Crystal structure of the high-P polymorph of Ca₂B₆O₆(OH)₁₀·2(H₂O) (meyerhofferite)

The crystal structure of the high-pressure polymorph of meyerhofferite, ideally Ca₂B₆O₆(OH)₁₀·2(H₂O), has been determined by means of single-crystal synchrotron X-ray diffraction data. Meyerhofferite undergoes a first-order isosymmetric phase transition to meyerhofferite-II, bracketed between 3.15 and 3.75 GPa, with a large volume discontinuity. The phase transition is marked by an increase in the coordination number of the boron B1 site, from III to IV, leading to a more interconnected and less compressible structure. The main structural differences between the two polymorphs and the P-induced deformation mechanisms at the atomic scale are discussed.

Computing details

For all structures, data collection: CrysAlis PRO 1.171.39.46 (Rigaku OD, 2018); cell refinement: CrysAlis PRO 1.171.39.46 (Rigaku OD, 2018); data reduction: CrysAlis PRO 1.171.39.46 (Rigaku OD, 2018); program(s) used to solve structure: Olex2 (Dolomanov et al., 2009); program(s) used to refine structure: Jana2006 (Petricek et al., 2014).

(I_0.0001GPa)

Crystal data

H7B3CaO9	Z = 2
Mr = 223.6	F(000) = 214
Triclinic, P1	Dx = 2.117 Mg m^−3
Hall symbol: -P 1	Synchrotron radiation, λ = 0.41066 Å
a = 6.639 (2) Å	Cell parameters from 767 reflections
b = 8.3489 (2) Å	θ = 2.3–19.0°
c = 6.4786 (2) Å	µ = 0.21 mm^−1
α = 90.770 (2)°	T = 293 K
β = 101.94 (1)°	Prismatic habit, colourless
γ = 86.747 (8)°	0.02 × 0.01 × 0.01 mm
V = 350.76 (11) Å^3

Data collection

Beamline diffractometer	493 reflections with I > 3σ(I)
Radiation source: ESRF: Synchrotron radiation, undulator, IVU20c	Rint = 0.010
Silicon monochromator	θmax = 19.3°, θmin = 2.3°
ω scans	h = −4→3
767 measured reflections	k = −12→12
522 independent reflections	l = −9→9

Refinement

Refinement on F	0 constraints
R[F^2 > 2σ(F^2)] = 0.050	H-atom parameters not defined
wR(F^2) = 0.068	Weighting scheme based on measured s.u.'s w = 1/(σ^2(F) + 0.0001F^2)
S = 4.10	(Δ/σ)max = 0.008
522 reflections	Δρmax = 0.33 e Å^−3
53 parameters	Δρmin = −0.22 e Å^−3
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ca	0.0115 (4)	0.37607 (9)	0.24452 (14)	0.0143 (3)*
B1	0.311 (3)	0.7984 (5)	0.4840 (9)	0.0153 (9)*
B2	0.278 (3)	0.6341 (6)	0.1633 (9)	0.0156 (10)*
B3	0.042 (2)	0.2644 (5)	0.6997 (8)	0.0151 (9)*
O1	0.4062 (17)	0.7351 (4)	0.3282 (6)	0.0200 (7)*
O2	0.4294 (16)	0.8873 (4)	0.6479 (6)	0.0195 (7)*
O3	0.1144 (16)	0.7781 (4)	0.4910 (6)	0.0171 (7)*
O4	0.3346 (16)	0.4609 (4)	0.2050 (5)	0.0201 (7)*
O5	0.0595 (19)	0.6517 (4)	0.1479 (6)	0.0159 (7)*
O6	0.1744 (16)	0.3795 (4)	0.6199 (5)	0.0164 (6)*
O7	0.1520 (16)	0.1061 (4)	0.2114 (5)	0.0199 (7)*
O8	0.1546 (17)	0.1222 (4)	0.7978 (6)	0.0196 (7)*
O9	0.3295 (17)	0.6713 (4)	0.9567 (5)	0.0180 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
?	?	?	?	?	?	?

Geometric parameters (Å, º)

Ca—B2	2.983 (14)	B3—O6	1.501 (14)
Ca—B2^i	2.932 (10)	B3—O8	1.446 (9)
Ca—O3^ii	2.463 (7)	O1—O2	2.398 (5)
Ca—O4	2.361 (11)	O1—O3	2.398 (14)
Ca—O5	2.448 (4)	O1—O4	2.453 (5)
Ca—O5^i	2.498 (4)	O1—O5	2.489 (14)
Ca—O6	2.449 (4)	O1—O6^iv	2.846 (14)
Ca—O6^ii	2.564 (6)	O1—O9^iii	2.413 (5)
Ca—O7	2.414 (5)	O2—O3	2.356 (13)
Ca—O9^ii	2.418 (10)	O2—O7^iv	2.743 (14)
B1—B2	2.453 (8)	O2—O8^v	2.897 (11)
B1—B3^ii	2.48 (2)	O2—O9	2.912 (8)
B1—O1	1.381 (13)	O3—O5	2.416 (5)
B1—O2	1.412 (10)	O3—O6^ii	2.370 (12)
B1—O3	1.34 (2)	O3—O7^ii	2.991 (11)
B1—O5	2.773 (11)	O3—O8^ii	2.423 (9)
B2—B3^ii	2.57 (2)	O4—O5	2.327 (12)
B2—O1	1.502 (11)	O4—O9^iii	2.391 (5)
B2—O3	2.806 (13)	O4—O9^iv	2.819 (13)
B2—O4	1.487 (7)	O5—O6^ii	2.401 (13)
B2—O5	1.43 (2)	O5—O8^ii	2.365 (10)
B2—O9^iii	1.489 (12)	O5—O9^iii	2.394 (15)
B3—O1^ii	2.95 (2)	O6—O8	2.474 (5)
B3—O3^ii	1.495 (12)	O7—O8^iii	2.688 (6)
B3—O5^ii	1.459 (13)	O7—O8^vi	2.858 (12)
B2—Ca—B2^i	100.6 (3)	B1—O3—B3^ii	122.5 (7)
B2—Ca—O3^ii	147.01 (18)	B1—O3—O1	28.6 (3)
B2—Ca—O4	29.5 (3)	B1—O3—O2	32.0 (3)
B2—Ca—O5	28.5 (4)	B1—O3—O5	90.6 (5)
B2—Ca—O5^i	83.3 (2)	B1—O3—O6^ii	146.2 (4)
B2—Ca—O6	90.1 (2)	B1—O3—O7^ii	132.9 (4)
B2—Ca—O6^ii	79.9 (3)	B1—O3—O8^ii	118.9 (4)
B2—Ca—O7	114.9 (4)	B2—O3—B3^ii	65.2 (7)
B2—Ca—O9^ii	125.8 (2)	B2—O3—O1	32.4 (4)
B2^i—Ca—O3^ii	110.1 (3)	B2—O3—O2	92.9 (5)
B2^i—Ca—O4	111.2 (3)	B2—O3—O5	30.7 (5)
B2^i—Ca—O5	85.2 (2)	B2—O3—O6^ii	87.0 (4)
B2^i—Ca—O5^i	29.2 (4)	B2—O3—O7^ii	166.2 (5)
B2^i—Ca—O6	165.6 (4)	B2—O3—O8^ii	83.0 (3)
B2^i—Ca—O6^ii	94.5 (3)	B3^ii—O3—O1	95.6 (6)
B2^i—Ca—O7	93.6 (2)	B3^ii—O3—O2	151.0 (7)
B2^i—Ca—O9^ii	30.4 (4)	B3^ii—O3—O5	34.7 (6)
O3^ii—Ca—O4	135.7 (2)	B3^ii—O3—O6^ii	37.8 (5)
O3^ii—Ca—O5	141.5 (2)	B3^ii—O3—O7^ii	101.8 (7)
O3^ii—Ca—O5^i	129.7 (2)	B3^ii—O3—O8^ii	33.9 (3)
O3^ii—Ca—O6	57.7 (3)	O1—O3—O2	60.6 (3)
O3^ii—Ca—O6^ii	85.8 (2)	O1—O3—O5	62.3 (4)
O3^ii—Ca—O7	75.6 (2)	O1—O3—O6^ii	118.8 (3)
O3^ii—Ca—O9^ii	81.2 (2)	O1—O3—O7^ii	161.5 (3)
O4—Ca—O5	57.8 (3)	O1—O3—O8^ii	102.9 (3)
O4—Ca—O5^i	84.6 (3)	O2—O3—O5	122.4 (5)
O4—Ca—O6	82.9 (3)	O2—O3—O6^ii	167.7 (2)
O4—Ca—O6^ii	106.1 (2)	O2—O3—O7^ii	100.9 (2)
O4—Ca—O7	86.4 (3)	O2—O3—O8^ii	130.1 (3)
O4—Ca—O9^ii	141.56 (18)	O5—O3—O6^ii	60.2 (3)
O5—Ca—O5^i	80.34 (13)	O5—O3—O7^ii	135.9 (5)
O5—Ca—O6	100.24 (15)	O5—O3—O8^ii	58.5 (3)
O5—Ca—O6^ii	57.2 (3)	O6^ii—O3—O7^ii	79.4 (4)
O5—Ca—O7	140.4 (3)	O6^ii—O3—O8^ii	62.1 (3)
O5—Ca—O9^ii	102.6 (3)	O7^ii—O3—O8^ii	88.4 (4)
O5^i—Ca—O6	164.7 (4)	Ca—O4—B2	99.2 (9)
O5^i—Ca—O6^ii	114.47 (19)	Ca—O4—O1	114.5 (4)
O5^i—Ca—O7	79.80 (15)	Ca—O4—O5	63.0 (4)
O5^i—Ca—O9^ii	58.3 (3)	Ca—O4—O9^iii	116.6 (4)
O6—Ca—O6^ii	77.68 (19)	Ca—O4—O9^iv	136.34 (18)
O6—Ca—O7	90.60 (15)	B2—O4—O1	35.0 (5)
O6—Ca—O9^ii	135.4 (3)	B2—O4—O5	36.4 (8)
O6^ii—Ca—O7	161.4 (2)	B2—O4—O9^iii	36.5 (5)
O6^ii—Ca—O9^ii	83.3 (2)	B2—O4—O9^iv	116.7 (8)
O7—Ca—O9^ii	95.5 (2)	O1—O4—O5	62.7 (3)
B2—B1—B3^ii	62.7 (6)	O1—O4—O9^iii	59.73 (15)
B2—B1—O1	33.2 (6)	O1—O4—O9^iv	109.1 (5)
B2—B1—O2	151.4 (12)	O5—O4—O9^iii	61.0 (3)
B2—B1—O3	90.6 (6)	O5—O4—O9^iv	144.4 (3)
B2—B1—O5	31.1 (5)	O9^iii—O4—O9^iv	84.6 (3)
B3^ii—B1—O1	95.0 (6)	Ca—O5—Ca^i	99.66 (14)
B3^ii—B1—O2	145.4 (10)	Ca—O5—B1	109.32 (19)
B3^ii—B1—O3	30.5 (4)	Ca—O5—B2	97.0 (3)
B3^ii—B1—O5	31.6 (3)	Ca—O5—B3^ii	98.5 (5)
O1—B1—O2	118.3 (13)	Ca—O5—O1	110.3 (3)
O1—B1—O3	123.8 (8)	Ca—O5—O3	100.34 (19)
O1—B1—O5	63.6 (5)	Ca—O5—O4	59.2 (2)
O2—B1—O3	117.9 (9)	Ca—O5—O6^ii	63.8 (2)
O2—B1—O5	174.5 (5)	Ca—O5—O8^ii	125.0 (5)
O3—B1—O5	60.6 (4)	Ca—O5—O9^iii	113.3 (3)
Ca—B2—Ca^i	79.4 (4)	Ca^i—O5—B1	142.8 (5)
Ca—B2—B1	102.9 (5)	Ca^i—O5—B2	92.4 (4)
Ca—B2—B3^ii	65.6 (4)	Ca^i—O5—B3^ii	135.4 (6)
Ca—B2—O1	125.9 (5)	Ca^i—O5—O1	117.9 (4)
Ca—B2—O3	80.3 (4)	Ca^i—O5—O3	159.43 (16)
Ca—B2—O4	51.4 (6)	Ca^i—O5—O4	94.6 (3)
Ca—B2—O5	54.5 (4)	Ca^i—O5—O6^ii	127.8 (5)
Ca—B2—O9^iii	126.1 (5)	Ca^i—O5—O8^ii	103.1 (2)
Ca^i—B2—B1	136.1 (6)	Ca^i—O5—O9^iii	59.2 (2)
Ca^i—B2—B3^ii	83.8 (5)	B1—O5—B2	62.0 (5)
Ca^i—B2—O1	147.3 (3)	B1—O5—B3^ii	63.2 (7)
Ca^i—B2—O3	114.8 (6)	B1—O5—O1	29.8 (4)
Ca^i—B2—O4	101.8 (4)	B1—O5—O3	28.8 (4)
Ca^i—B2—O5	58.3 (4)	B1—O5—O4	81.3 (4)
Ca^i—B2—O9^iii	55.3 (5)	B1—O5—O6^ii	86.6 (4)
B1—B2—B3^ii	59.3 (5)	B1—O5—O8^ii	79.1 (3)
B1—B2—O1	30.2 (6)	B1—O5—O9^iii	87.6 (5)
B1—B2—O3	28.5 (5)	B2—O5—B3^ii	125.2 (7)
B1—B2—O4	113.7 (4)	B2—O5—O1	32.9 (3)
B1—B2—O5	86.9 (7)	B2—O5—O3	89.9 (5)
B1—B2—O9^iii	129.4 (6)	B2—O5—O4	38.0 (3)
B3^ii—B2—O1	88.7 (7)	B2—O5—O6^ii	136.4 (4)
B3^ii—B2—O3	31.9 (3)	B2—O5—O8^ii	130.8 (4)
B3^ii—B2—O4	113.6 (9)	B2—O5—O9^iii	35.8 (4)
B3^ii—B2—O5	27.7 (3)	B3^ii—O5—O1	92.8 (6)
B3^ii—B2—O9^iii	127.2 (8)	B3^ii—O5—O3	35.6 (6)
O1—B2—O3	58.7 (6)	B3^ii—O5—O4	129.4 (4)
O1—B2—O4	110.4 (8)	B3^ii—O5—O6^ii	36.4 (5)
O1—B2—O5	116.0 (8)	B3^ii—O5—O8^ii	35.3 (3)
O1—B2—O9^iii	107.6 (10)	B3^ii—O5—O9^iii	142.9 (6)
O3—B2—O4	111.4 (5)	O1—O5—O3	58.5 (3)
O3—B2—O5	59.4 (5)	O1—O5—O4	61.1 (3)
O3—B2—O9^iii	141.6 (4)	O1—O5—O6^ii	114.1 (3)
O4—B2—O5	105.6 (10)	O1—O5—O8^ii	101.9 (3)
O4—B2—O9^iii	107.0 (7)	O1—O5—O9^iii	59.2 (3)
O5—B2—O9^iii	110.0 (8)	O3—O5—O4	99.7 (3)
B1^ii—B3—B2^ii	58.0 (5)	O3—O5—O6^ii	58.9 (3)
B1^ii—B3—O1^ii	27.8 (3)	O3—O5—O8^ii	60.9 (2)
B1^ii—B3—O3^ii	27.0 (5)	O3—O5—O9^iii	116.0 (5)
B1^ii—B3—O5^ii	85.2 (9)	O4—O5—O6^ii	112.8 (3)
B1^ii—B3—O6	124.7 (5)	O4—O5—O8^ii	160.1 (3)
B1^ii—B3—O8	110.7 (6)	O4—O5—O9^iii	60.9 (3)
B2^ii—B3—O1^ii	30.6 (3)	O6^ii—O5—O8^ii	62.5 (3)
B2^ii—B3—O3^ii	82.9 (8)	O6^ii—O5—O9^iii	172.1 (4)
B2^ii—B3—O5^ii	27.1 (6)	O8^ii—O5—O9^iii	121.5 (3)
B2^ii—B3—O6	120.8 (5)	Ca—O6—Ca^ii	102.3 (2)
B2^ii—B3—O8	117.2 (7)	Ca—O6—B3	99.0 (4)
O1^ii—B3—O3^ii	54.1 (6)	Ca—O6—O1^iv	109.3 (3)
O1^ii—B3—O5^ii	57.5 (7)	Ca—O6—O3^ii	61.44 (19)
O1^ii—B3—O6	131.9 (6)	Ca—O6—O5^ii	114.1 (4)
O1^ii—B3—O8	113.8 (8)	Ca—O6—O8	112.8 (2)
O3^ii—B3—O5^ii	109.7 (11)	Ca^ii—O6—B3	92.6 (5)
O3^ii—B3—O6	104.5 (5)	Ca^ii—O6—O1^iv	134.6 (3)
O3^ii—B3—O8	111.0 (4)	Ca^ii—O6—O3^ii	98.4 (4)
O5^ii—B3—O6	108.4 (5)	Ca^ii—O6—O5^ii	59.0 (2)
O5^ii—B3—O8	109.0 (5)	Ca^ii—O6—O8	115.8 (3)
O6—B3—O8	114.1 (12)	B3—O6—O1^iv	113.1 (5)
B1—O1—B2	116.5 (12)	B3—O6—O3^ii	37.6 (4)
B1—O1—B3^ii	57.1 (7)	B3—O6—O5^ii	35.2 (4)
B1—O1—O2	31.2 (7)	B3—O6—O8	32.2 (5)
B1—O1—O3	27.6 (7)	O1^iv—O6—O3^ii	125.1 (2)
B1—O1—O4	118.5 (7)	O1^iv—O6—O5^ii	128.6 (2)
B1—O1—O5	86.6 (8)	O1^iv—O6—O8	80.9 (3)
B1—O1—O6^iv	126.4 (7)	O3^ii—O6—O5^ii	60.8 (3)
B1—O1—O9^iii	140.4 (8)	O3^ii—O6—O8	60.0 (3)
B2—O1—B3^ii	60.6 (8)	O5^ii—O6—O8	58.0 (3)
B2—O1—O2	147.7 (10)	Ca—O7—O2^iv	106.6 (2)
B2—O1—O3	88.9 (8)	Ca—O7—O3^ii	52.92 (16)
B2—O1—O4	34.6 (3)	Ca—O7—O8^iii	96.47 (15)
B2—O1—O5	31.2 (7)	Ca—O7—O8^vi	111.1 (4)
B2—O1—O6^iv	108.3 (7)	O2^iv—O7—O3^ii	117.2 (2)
B2—O1—O9^iii	36.0 (5)	O2^iv—O7—O8^iii	96.5 (4)
B3^ii—O1—O2	88.0 (4)	O2^iv—O7—O8^vi	136.4 (2)
B3^ii—O1—O3	30.3 (2)	O3^ii—O7—O8^iii	138.6 (4)
B3^ii—O1—O4	78.7 (4)	O3^ii—O7—O8^vi	72.6 (3)
B3^ii—O1—O5	29.6 (2)	O8^iii—O7—O8^vi	100.1 (3)
B3^ii—O1—O6^iv	160.2 (2)	B3—O8—O2^vii	131.4 (5)
B3^ii—O1—O9^iii	85.7 (4)	B3—O8—O3^ii	35.2 (4)
O2—O1—O3	58.8 (3)	B3—O8—O5^ii	35.7 (4)
O2—O1—O4	138.2 (3)	B3—O8—O6	33.6 (7)
O2—O1—O5	117.6 (5)	B3—O8—O7^viii	112.4 (5)
O2—O1—O6^iv	99.1 (4)	B3—O8—O7^vi	104.8 (8)
O2—O1—O9^iii	159.8 (2)	O2^vii—O8—O3^ii	110.7 (2)
O3—O1—O4	96.7 (4)	O2^vii—O8—O5^ii	166.7 (3)
O3—O1—O5	59.2 (3)	O2^vii—O8—O6	107.8 (4)
O3—O1—O6^iv	146.4 (2)	O2^vii—O8—O7^viii	115.3 (2)
O3—O1—O9^iii	115.9 (5)	O2^vii—O8—O7^vi	92.1 (2)
O4—O1—O5	56.2 (3)	O3^ii—O8—O5^ii	60.6 (2)
O4—O1—O6^iv	83.8 (3)	O3^ii—O8—O6	57.9 (3)
O4—O1—O9^iii	58.86 (15)	O3^ii—O8—O7^viii	129.4 (5)
O5—O1—O6^iv	138.4 (2)	O3^ii—O8—O7^vi	78.3 (3)
O5—O1—O9^iii	58.4 (3)	O5^ii—O8—O6	59.4 (3)
O6^iv—O1—O9^iii	93.2 (4)	O5^ii—O8—O7^viii	76.9 (2)
B1—O2—O1	30.5 (7)	O5^ii—O8—O7^vi	95.5 (5)
B1—O2—O3	30.1 (7)	O6—O8—O7^viii	122.13 (16)
B1—O2—O7^iv	131.0 (8)	O6—O8—O7^vi	135.8 (4)
B1—O2—O8^v	108.1 (8)	O7^viii—O8—O7^vi	79.9 (3)
B1—O2—O9	89.8 (5)	Ca^ii—O9—B2^viii	94.2 (8)
O1—O2—O3	60.6 (3)	Ca^ii—O9—O1^viii	124.4 (5)
O1—O2—O7^iv	101.8 (4)	Ca^ii—O9—O2	94.8 (2)
O1—O2—O8^v	133.6 (4)	Ca^ii—O9—O4^viii	95.1 (4)
O1—O2—O9	106.0 (2)	Ca^ii—O9—O4^iv	116.75 (18)
O3—O2—O7^iv	157.0 (3)	Ca^ii—O9—O5^viii	62.5 (3)
O3—O2—O8^v	81.8 (4)	B2^viii—O9—O1^viii	36.4 (5)
O3—O2—O9	73.3 (3)	B2^viii—O9—O2	153.4 (3)
O7^iv—O2—O8^v	120.3 (2)	B2^viii—O9—O4^viii	36.5 (3)
O7^iv—O2—O9	100.2 (3)	B2^viii—O9—O4^iv	126.8 (7)
O8^v—O2—O9	86.0 (3)	B2^viii—O9—O5^viii	34.2 (7)
Ca^ii—O3—B1	126.7 (4)	O1^viii—O9—O2	120.9 (3)
Ca^ii—O3—B2	123.17 (19)	O1^viii—O9—O4^viii	61.41 (15)
Ca^ii—O3—B3^ii	98.7 (6)	O1^viii—O9—O4^iv	115.2 (4)
Ca^ii—O3—O1	132.2 (3)	O1^viii—O9—O5^viii	62.4 (3)
Ca^ii—O3—O2	109.6 (2)	O2—O9—O4^viii	164.8 (5)
Ca^ii—O3—O5	113.1 (3)	O2—O9—O4^iv	69.8 (3)
Ca^ii—O3—O6^ii	60.9 (2)	O2—O9—O5^viii	137.0 (4)
Ca^ii—O3—O7^ii	51.44 (17)	O4^viii—O9—O4^iv	95.4 (3)
Ca^ii—O3—O8^ii	114.1 (5)	O4^viii—O9—O5^viii	58.2 (3)
B1—O3—B2	60.9 (5)	O4^iv—O9—O5^viii	152.14 (18)

Symmetry codes: (i) −x, −y+1, −z; (ii) −x, −y+1, −z+1; (iii) x, y, z−1; (iv) −x+1, −y+1, −z+1; (v) x, y+1, z; (vi) −x, −y, −z+1; (vii) x, y−1, z; (viii) x, y, z+1.

(I_1.31GPa)

Crystal data

H7B3CaO9	Z = 2
Mr = 223.6	F(000) = 214
Triclinic, P1	Dx = 2.205 Mg m^−3
Hall symbol: -P 1	Synchrotron radiation, λ = 0.41066 Å
a = 6.550 (2) Å	Cell parameters from 755 reflections
b = 8.2005 (2) Å	θ = 2.4–19.3°
c = 6.4337 (2) Å	µ = 0.22 mm^−1
α = 90.367 (3)°	T = 293 K
β = 102.63 (1)°	Prismatic habit, colourless
γ = 86.784 (9)°	0.02 × 0.01 × 0.01 mm
V = 336.68 (10) Å^3

Data collection

Beamline diffractometer	465 reflections with I > 3σ(I)
Radiation source: ESRF: Synchrotron radiation, undulator, IVU20c	Rint = 0.010
Silicon monochromator	θmax = 19.3°, θmin = 2.2°
ω scans	h = −4→3
755 measured reflections	k = −12→12
503 independent reflections	l = −9→9

Refinement

Refinement on F	0 constraints
R[F^2 > 2σ(F^2)] = 0.052	H-atom parameters not defined
wR(F^2) = 0.068	Weighting scheme based on measured s.u.'s w = 1/(σ^2(F) + 0.0001F^2)
S = 3.99	(Δ/σ)max = 0.032
503 reflections	Δρmax = 0.35 e Å^−3
53 parameters	Δρmin = −0.28 e Å^−3
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ca	0.0110 (5)	0.37477 (11)	0.24538 (17)	0.0132 (3)*
B1	0.312 (3)	0.8029 (6)	0.4865 (10)	0.0140 (10)*
B2	0.283 (4)	0.6356 (7)	0.1664 (11)	0.0145 (11)*
B3	0.046 (3)	0.2632 (6)	0.7019 (10)	0.0148 (10)*
O1	0.4099 (19)	0.7380 (4)	0.3332 (7)	0.0180 (8)*
O2	0.4335 (18)	0.8925 (4)	0.6539 (6)	0.0165 (8)*
O3	0.113 (2)	0.7830 (4)	0.4917 (7)	0.0153 (8)*
O4	0.339 (2)	0.4597 (4)	0.2088 (7)	0.0186 (8)*
O5	0.060 (2)	0.6531 (4)	0.1472 (7)	0.0149 (8)*
O6	0.1769 (18)	0.3812 (4)	0.6228 (6)	0.0150 (7)*
O7	0.1531 (19)	0.1019 (4)	0.2140 (6)	0.0187 (8)*
O8	0.159 (2)	0.1199 (4)	0.8035 (7)	0.0179 (8)*
O9	0.3340 (19)	0.6753 (4)	0.9596 (6)	0.0166 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
?	?	?	?	?	?	?

Geometric parameters (Å, º)

Ca—B2	2.973 (16)	B3—O6	1.492 (17)
Ca—B2^i	2.918 (12)	B3—O8	1.435 (10)
Ca—B3^ii	2.998 (6)	O1—O2	2.394 (6)
Ca—O3^ii	2.439 (8)	O1—O3	2.393 (17)
Ca—O4	2.354 (13)	O1—O4	2.450 (6)
Ca—O5	2.429 (5)	O1—O5	2.479 (16)
Ca—O5^i	2.478 (4)	O1—O6^iv	2.781 (16)
Ca—O6	2.435 (5)	O1—O9^iii	2.404 (6)
Ca—O6^ii	2.529 (7)	O2—O2^v	2.959 (10)
Ca—O7	2.399 (6)	O2—O3	2.352 (15)
Ca—O9^ii	2.410 (11)	O2—O7^iv	2.658 (16)
B1—B2	2.446 (9)	O2—O8^vi	2.827 (13)
B1—B3^ii	2.48 (2)	O2—O9	2.864 (9)
B1—O1	1.379 (16)	O3—O5	2.417 (6)
B1—O2	1.420 (12)	O3—O6^ii	2.374 (14)
B1—O3	1.33 (2)	O3—O7^ii	2.960 (14)
B1—O5	2.759 (13)	O3—O8^ii	2.409 (11)
B2—B3^ii	2.57 (3)	O4—O5	2.320 (14)
B2—O1	1.492 (13)	O4—O9^iii	2.389 (6)
B2—O3	2.812 (16)	O4—O9^iv	2.779 (15)
B2—O4	1.481 (7)	O5—O6^ii	2.394 (16)
B2—O5	1.44 (3)	O5—O8^ii	2.348 (12)
B2—O9^iii	1.483 (14)	O5—O9^iii	2.388 (17)
B3—O1^ii	2.94 (2)	O6—O8	2.465 (6)
B3—O3^ii	1.500 (14)	O7—O8^iii	2.655 (7)
B3—O5^ii	1.457 (16)	O7—O8^vii	2.796 (14)
B2—Ca—B2^i	101.0 (3)	O8^vi—O2—O9	84.7 (3)
B2—Ca—B3^ii	51.1 (5)	Ca^ii—O3—B1	126.4 (5)
B2—Ca—O3^ii	147.0 (2)	Ca^ii—O3—B2	122.6 (2)
B2—Ca—O4	29.5 (4)	Ca^ii—O3—B3^ii	98.1 (7)
B2—Ca—O5	28.7 (5)	Ca^ii—O3—O1	131.4 (3)
B2—Ca—O5^i	83.3 (3)	Ca^ii—O3—O2	109.2 (2)
B2—Ca—O6	89.3 (3)	Ca^ii—O3—O5	112.8 (3)
B2—Ca—O6^ii	80.5 (4)	Ca^ii—O3—O6^ii	60.8 (3)
B2—Ca—O7	114.5 (4)	Ca^ii—O3—O7^ii	51.7 (2)
B2—Ca—O9^ii	126.5 (3)	Ca^ii—O3—O8^ii	114.1 (6)
B2^i—Ca—B3^ii	95.1 (2)	B1—O3—B2	60.4 (6)
B2^i—Ca—O3^ii	110.0 (4)	B1—O3—B3^ii	122.3 (9)
B2^i—Ca—O4	111.3 (4)	B1—O3—O1	28.4 (4)
B2^i—Ca—O5	85.4 (2)	B1—O3—O2	32.2 (4)
B2^i—Ca—O5^i	29.5 (5)	B1—O3—O5	90.1 (6)
B2^i—Ca—O6	165.7 (5)	B1—O3—O6^ii	145.2 (5)
B2^i—Ca—O6^ii	94.5 (3)	B1—O3—O7^ii	133.0 (4)
B2^i—Ca—O7	93.4 (2)	B1—O3—O8^ii	119.1 (5)
B2^i—Ca—O9^ii	30.5 (4)	B2—O3—B3^ii	65.3 (8)
B3^ii—Ca—O3^ii	113.4 (3)	B2—O3—O1	32.0 (4)
B3^ii—Ca—O4	78.9 (4)	B2—O3—O2	92.6 (6)
B3^ii—Ca—O5	28.8 (4)	B2—O3—O5	30.8 (5)
B3^ii—Ca—O5^i	102.12 (15)	B2—O3—O6^ii	86.7 (4)
B3^ii—Ca—O6	83.49 (17)	B2—O3—O7^ii	166.6 (6)
B3^ii—Ca—O6^ii	29.8 (4)	B2—O3—O8^ii	82.9 (4)
B3^ii—Ca—O7	164.6 (5)	B3^ii—O3—O1	95.5 (8)
B3^ii—Ca—O9^ii	98.8 (3)	B3^ii—O3—O2	151.5 (8)
O3^ii—Ca—O4	135.3 (3)	B3^ii—O3—O5	34.6 (7)
O3^ii—Ca—O5	142.0 (2)	B3^ii—O3—O6^ii	37.4 (5)
O3^ii—Ca—O5^i	129.6 (3)	B3^ii—O3—O7^ii	102.3 (9)
O3^ii—Ca—O6	58.3 (3)	B3^ii—O3—O8^ii	34.0 (3)
O3^ii—Ca—O6^ii	85.9 (2)	O1—O3—O2	60.6 (4)
O3^ii—Ca—O7	75.4 (3)	O1—O3—O5	62.0 (4)
O3^ii—Ca—O9^ii	81.0 (3)	O1—O3—O6^ii	118.1 (3)
O4—Ca—O5	58.0 (4)	O1—O3—O7^ii	161.3 (4)
O4—Ca—O5^i	84.4 (3)	O1—O3—O8^ii	102.9 (4)
O4—Ca—O6	82.5 (3)	O2—O3—O5	122.2 (6)
O4—Ca—O6^ii	106.8 (3)	O2—O3—O6^ii	166.7 (3)
O4—Ca—O7	86.0 (3)	O2—O3—O7^ii	100.8 (3)
O4—Ca—O9^ii	141.8 (2)	O2—O3—O8^ii	131.0 (3)
O5—Ca—O5^i	80.34 (15)	O5—O3—O6^ii	60.0 (4)
O5—Ca—O6	99.54 (18)	O5—O3—O7^ii	136.4 (6)
O5—Ca—O6^ii	57.7 (3)	O5—O3—O8^ii	58.2 (3)
O5—Ca—O7	140.1 (4)	O6^ii—O3—O7^ii	80.1 (4)
O5—Ca—O9^ii	103.1 (3)	O6^ii—O3—O8^ii	62.0 (3)
O5^i—Ca—O6	164.5 (4)	O7^ii—O3—O8^ii	89.1 (4)
O5^i—Ca—O6^ii	114.8 (2)	Ca—O4—B2	99.1 (11)
O5^i—Ca—O7	79.39 (17)	Ca—O4—O1	113.9 (5)
O5^i—Ca—O9^ii	58.5 (4)	Ca—O4—O5	62.6 (4)
O6—Ca—O6^ii	77.2 (2)	Ca—O4—O9^iii	116.5 (5)
O6—Ca—O7	91.40 (18)	Ca—O4—O9^iv	135.4 (2)
O6—Ca—O9^ii	135.6 (3)	B2—O4—O1	34.7 (5)
O6^ii—Ca—O7	161.3 (3)	B2—O4—O5	36.7 (10)
O6^ii—Ca—O9^ii	83.4 (3)	B2—O4—O9^iii	36.3 (6)
O7—Ca—O9^ii	95.0 (3)	B2—O4—O9^iv	116.6 (10)
B2—B1—B3^ii	63.1 (7)	O1—O4—O5	62.6 (4)
B2—B1—O1	33.0 (7)	O1—O4—O9^iii	59.57 (17)
B2—B1—O2	150.5 (14)	O1—O4—O9^iv	110.6 (5)
B2—B1—O3	91.5 (8)	O5—O4—O9^iii	60.9 (4)
B2—B1—O5	31.4 (6)	O5—O4—O9^iv	143.4 (3)
B3^ii—B1—O1	95.3 (7)	O9^iii—O4—O9^iv	84.2 (4)
B3^ii—B1—O2	146.1 (11)	Ca—O5—Ca^i	99.66 (16)
B3^ii—B1—O3	30.8 (4)	Ca—O5—B1	109.5 (2)
B3^ii—B1—O5	31.7 (4)	Ca—O5—B2	97.2 (4)
O1—B1—O2	117.6 (15)	Ca—O5—B3^ii	97.8 (6)
O1—B1—O3	124.5 (9)	Ca—O5—O1	110.3 (3)
O1—B1—O5	63.7 (6)	Ca—O5—O3	100.5 (2)
O2—B1—O3	117.9 (10)	Ca—O5—O4	59.4 (3)
O2—B1—O5	175.3 (5)	Ca—O5—O6^ii	63.3 (3)
O3—B1—O5	61.2 (5)	Ca—O5—O8^ii	124.4 (6)
Ca—B2—Ca^i	79.0 (4)	Ca—O5—O9^iii	113.7 (4)
Ca—B2—B1	102.5 (6)	Ca^i—O5—B1	143.0 (6)
Ca—B2—B3^ii	65.0 (5)	Ca^i—O5—B2	92.5 (5)
Ca—B2—O1	125.5 (6)	Ca^i—O5—B3^ii	135.4 (8)
Ca—B2—O3	80.1 (5)	Ca^i—O5—O1	118.1 (5)
Ca—B2—O4	51.4 (8)	Ca^i—O5—O3	159.20 (18)
Ca—B2—O5	54.2 (5)	Ca^i—O5—O4	94.4 (3)
Ca—B2—O9^iii	126.4 (6)	Ca^i—O5—O6^ii	127.8 (6)
Ca^i—B2—B1	135.4 (8)	Ca^i—O5—O8^ii	103.1 (3)
Ca^i—B2—B3^ii	83.3 (6)	Ca^i—O5—O9^iii	59.4 (3)
Ca^i—B2—O1	147.3 (4)	B1—O5—B2	62.2 (5)
Ca^i—B2—O3	114.3 (7)	B1—O5—B3^ii	63.4 (8)
Ca^i—B2—O4	101.3 (5)	B1—O5—O1	29.9 (4)
Ca^i—B2—O5	58.0 (4)	B1—O5—O3	28.7 (5)
Ca^i—B2—O9^iii	55.5 (6)	B1—O5—O4	81.8 (5)
B1—B2—B3^ii	59.0 (6)	B1—O5—O6^ii	86.6 (4)
B1—B2—O1	30.2 (7)	B1—O5—O8^ii	79.1 (4)
B1—B2—O3	28.1 (5)	B1—O5—O9^iii	87.6 (6)
B1—B2—O4	114.4 (4)	B2—O5—B3^ii	125.5 (8)
B1—B2—O5	86.4 (8)	B2—O5—O1	32.9 (4)
B1—B2—O9^iii	129.1 (7)	B2—O5—O3	90.0 (5)
B3^ii—B2—O1	88.6 (8)	B2—O5—O4	38.0 (4)
B3^ii—B2—O3	32.0 (4)	B2—O5—O6^ii	136.1 (4)
B3^ii—B2—O4	113.1 (11)	B2—O5—O8^ii	131.2 (5)
B3^ii—B2—O5	27.4 (4)	B2—O5—O9^iii	35.8 (4)
B3^ii—B2—O9^iii	126.7 (9)	B3^ii—O5—O1	93.2 (7)
O1—B2—O3	58.3 (7)	B3^ii—O5—O3	35.8 (7)
O1—B2—O4	111.0 (9)	B3^ii—O5—O4	129.6 (5)
O1—B2—O5	115.5 (10)	B3^ii—O5—O6^ii	36.2 (5)
O1—B2—O9^iii	107.8 (12)	B3^ii—O5—O8^ii	35.4 (3)
O3—B2—O4	111.8 (7)	B3^ii—O5—O9^iii	143.2 (7)
O3—B2—O5	59.3 (5)	O1—O5—O3	58.5 (4)
O3—B2—O9^iii	140.7 (4)	O1—O5—O4	61.3 (4)
O4—B2—O5	105.3 (11)	O1—O5—O6^ii	114.0 (3)
O4—B2—O9^iii	107.4 (9)	O1—O5—O8^ii	102.2 (3)
O5—B2—O9^iii	109.6 (9)	O1—O5—O9^iii	59.2 (4)
Ca^ii—B3—B1^ii	101.1 (5)	O3—O5—O4	100.1 (4)
Ca^ii—B3—B2^ii	64.0 (3)	O3—O5—O6^ii	59.1 (4)
Ca^ii—B3—O1^ii	85.4 (4)	O3—O5—O8^ii	60.7 (3)
Ca^ii—B3—O3^ii	107.1 (5)	O3—O5—O9^iii	115.8 (6)
Ca^ii—B3—O5^ii	53.4 (3)	O4—O5—O6^ii	112.6 (3)
Ca^ii—B3—O6	57.4 (3)	O4—O5—O8^ii	160.5 (4)
Ca^ii—B3—O8	142.4 (6)	O4—O5—O9^iii	61.0 (4)
B1^ii—B3—B2^ii	57.9 (6)	O6^ii—O5—O8^ii	62.6 (4)
B1^ii—B3—O1^ii	27.8 (4)	O6^ii—O5—O9^iii	171.9 (5)
B1^ii—B3—O3^ii	26.9 (7)	O8^ii—O5—O9^iii	121.6 (3)
B1^ii—B3—O5^ii	84.9 (10)	Ca—O6—Ca^ii	102.8 (3)
B1^ii—B3—O6	124.6 (5)	Ca—O6—B3	98.5 (5)
B1^ii—B3—O8	110.4 (8)	Ca—O6—O1^iv	107.5 (3)
B2^ii—B3—O1^ii	30.4 (4)	Ca—O6—O3^ii	60.9 (2)
B2^ii—B3—O3^ii	82.8 (10)	Ca—O6—O5^ii	113.7 (5)
B2^ii—B3—O5^ii	27.0 (7)	Ca—O6—O8	112.2 (3)
B2^ii—B3—O6	120.6 (6)	Ca^ii—O6—B3	92.8 (7)
B2^ii—B3—O8	116.9 (9)	Ca^ii—O6—O1^iv	136.5 (3)
O1^ii—B3—O3^ii	54.0 (8)	Ca^ii—O6—O3^ii	98.9 (5)
O1^ii—B3—O5^ii	57.2 (8)	Ca^ii—O6—O5^ii	59.1 (2)
O1^ii—B3—O6	131.5 (7)	Ca^ii—O6—O8	115.6 (4)
O1^ii—B3—O8	113.6 (9)	B3—O6—O1^iv	112.3 (6)
O3^ii—B3—O5^ii	109.6 (14)	B3—O6—O3^ii	37.6 (4)
O3^ii—B3—O6	105.0 (6)	B3—O6—O5^ii	35.3 (4)
O3^ii—B3—O8	110.3 (5)	B3—O6—O8	31.9 (6)
O5^ii—B3—O6	108.5 (5)	O1^iv—O6—O3^ii	122.9 (3)
O5^ii—B3—O8	108.6 (6)	O1^iv—O6—O5^ii	129.4 (3)
O6—B3—O8	114.8 (14)	O1^iv—O6—O8	80.6 (4)
B1—O1—B2	116.8 (14)	O3^ii—O6—O5^ii	60.9 (4)
B1—O1—B3^ii	56.9 (8)	O3^ii—O6—O8	59.7 (3)
B1—O1—O2	31.7 (8)	O5^ii—O6—O8	57.8 (3)
B1—O1—O3	27.2 (8)	Ca—O7—O2^iv	107.0 (3)
B1—O1—O4	118.9 (8)	Ca—O7—O3^ii	52.89 (19)
B1—O1—O5	86.4 (9)	Ca—O7—O8^iii	96.72 (17)
B1—O1—O6^iv	128.9 (7)	Ca—O7—O8^vii	109.9 (5)
B1—O1—O9^iii	140.0 (10)	O2^iv—O7—O3^ii	118.4 (3)
B2—O1—B3^ii	61.0 (9)	O2^iv—O7—O8^iii	94.5 (5)
B2—O1—O2	148.4 (11)	O2^iv—O7—O8^vii	138.2 (3)
B2—O1—O3	89.6 (10)	O3^ii—O7—O8^iii	139.3 (4)
B2—O1—O4	34.4 (4)	O3^ii—O7—O8^vii	72.2 (3)
B2—O1—O5	31.6 (9)	O8^iii—O7—O8^vii	100.0 (3)
B2—O1—O6^iv	105.9 (9)	B3—O8—O2^viii	129.9 (6)
B2—O1—O9^iii	36.0 (6)	B3—O8—O3^ii	35.7 (4)
B3^ii—O1—O2	88.3 (5)	B3—O8—O5^ii	36.0 (5)
B3^ii—O1—O3	30.5 (3)	B3—O8—O6	33.3 (8)
B3^ii—O1—O4	78.6 (4)	B3—O8—O7^ix	112.6 (6)
B3^ii—O1—O5	29.6 (3)	B3—O8—O7^vii	103.3 (9)
B3^ii—O1—O6^iv	159.2 (2)	O2^viii—O8—O3^ii	109.3 (3)
B3^ii—O1—O9^iii	85.8 (4)	O2^viii—O8—O5^ii	165.5 (3)
O2—O1—O3	58.9 (4)	O2^viii—O8—O6	106.5 (4)
O2—O1—O4	138.5 (3)	O2^viii—O8—O7^ix	116.6 (3)
O2—O1—O5	117.9 (6)	O2^viii—O8—O7^vii	93.9 (3)
O2—O1—O6^iv	101.0 (4)	O3^ii—O8—O5^ii	61.1 (3)
O2—O1—O9^iii	159.6 (3)	O3^ii—O8—O6	58.3 (3)
O3—O1—O4	97.2 (5)	O3^ii—O8—O7^ix	129.3 (6)
O3—O1—O5	59.4 (4)	O3^ii—O8—O7^vii	76.3 (4)
O3—O1—O6^iv	148.0 (2)	O5^ii—O8—O6	59.6 (3)
O3—O1—O9^iii	116.1 (6)	O5^ii—O8—O7^ix	76.8 (3)
O4—O1—O5	56.2 (4)	O5^ii—O8—O7^vii	93.9 (5)
O4—O1—O6^iv	82.2 (4)	O6—O8—O7^ix	122.44 (19)
O4—O1—O9^iii	58.96 (17)	O6—O8—O7^vii	134.1 (5)
O5—O1—O6^iv	136.5 (3)	O7^ix—O8—O7^vii	80.0 (3)
O5—O1—O9^iii	58.5 (4)	Ca^ii—O9—B2^ix	94.1 (10)
O6^iv—O1—O9^iii	91.2 (4)	Ca^ii—O9—O1^ix	124.0 (6)
B1—O2—O1	30.7 (8)	Ca^ii—O9—O2	95.2 (2)
B1—O2—O2^v	91.5 (5)	Ca^ii—O9—O4^ix	94.4 (4)
B1—O2—O3	29.9 (8)	Ca^ii—O9—O4^iv	114.7 (2)
B1—O2—O7^iv	130.2 (9)	Ca^ii—O9—O5^ix	62.2 (4)
B1—O2—O8^vi	107.7 (9)	B2^ix—O9—O1^ix	36.2 (6)
B1—O2—O9	90.0 (5)	B2^ix—O9—O2	153.9 (3)
O1—O2—O2^v	73.8 (2)	B2^ix—O9—O4^ix	36.3 (4)
O1—O2—O3	60.6 (4)	B2^ix—O9—O4^iv	127.5 (8)
O1—O2—O7^iv	100.6 (5)	B2^ix—O9—O5^ix	34.6 (9)
O1—O2—O8^vi	134.0 (5)	O1^ix—O9—O2	121.2 (3)
O1—O2—O9	105.9 (2)	O1^ix—O9—O4^ix	61.47 (17)
O2^v—O2—O3	109.3 (3)	O1^ix—O9—O4^iv	117.3 (5)
O2^v—O2—O7^iv	75.1 (4)	O1^ix—O9—O5^ix	62.3 (4)
O2^v—O2—O8^vi	98.4 (2)	O2—O9—O4^ix	164.7 (6)
O2^v—O2—O9	176.0 (5)	O2—O9—O4^iv	69.4 (3)
O3—O2—O7^iv	156.5 (3)	O2—O9—O5^ix	137.2 (4)
O3—O2—O8^vi	81.3 (4)	O4^ix—O9—O4^iv	95.8 (4)
O3—O2—O9	73.5 (3)	O4^ix—O9—O5^ix	58.1 (4)
O7^iv—O2—O8^vi	121.5 (3)	O4^iv—O9—O5^ix	151.8 (2)
O7^iv—O2—O9	101.2 (3)

Symmetry codes: (i) −x, −y+1, −z; (ii) −x, −y+1, −z+1; (iii) x, y, z−1; (iv) −x+1, −y+1, −z+1; (v) −x+1, −y+2, −z+1; (vi) x, y+1, z; (vii) −x, −y, −z+1; (viii) x, y−1, z; (ix) x, y, z+1.

(I_2.95GPa)

Crystal data

H7B3CaO9	Z = 2
Mr = 223.6	F(000) = 214
Triclinic, P1	Dx = 2.286 Mg m^−3
Hall symbol: -P 1	Synchrotron radiation, λ = 0.41066 Å
a = 6.478 (3) Å	Cell parameters from 717 reflections
b = 8.0733 (2) Å	θ = 2.4–19.6°
c = 6.3923 (2) Å	µ = 0.23 mm^−1
α = 89.972 (3)°	T = 293 K
β = 103.30 (1)°	Prismatic habit, colourless
γ = 86.857 (9)°	0.02 × 0.01 × 0.01 mm
V = 324.82 (15) Å^3

Data collection

Beamline diffractometer	449 reflections with I > 3σ(I)
Radiation source: ESRF: Synchrotron radiation, undulator, IVU20c	Rint = 0.014
Silicon monochromator	θmax = 19.6°, θmin = 2.4°
ω scans	h = −4→2
717 measured reflections	k = −12→12
489 independent reflections	l = −9→9

Refinement

Refinement on F	0 constraints
R[F^2 > 2σ(F^2)] = 0.048	H-atom parameters not defined
wR(F^2) = 0.063	Weighting scheme based on measured s.u.'s w = 1/(σ^2(F) + 0.0001F^2)
S = 3.35	(Δ/σ)max = 0.015
489 reflections	Δρmax = 0.37 e Å^−3
53 parameters	Δρmin = −0.28 e Å^−3
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ca	0.0102 (5)	0.37356 (10)	0.24588 (16)	0.0122 (3)*
B1	0.311 (3)	0.8059 (6)	0.4900 (10)	0.0133 (10)*
B2	0.293 (4)	0.6355 (6)	0.1708 (10)	0.0141 (11)*
B3	0.050 (3)	0.2622 (6)	0.7042 (10)	0.0138 (10)*
O1	0.4136 (18)	0.7400 (4)	0.3379 (6)	0.0165 (7)*
O2	0.4360 (17)	0.8967 (4)	0.6584 (6)	0.0154 (7)*
O3	0.1090 (19)	0.7867 (4)	0.4906 (6)	0.0138 (7)*
O4	0.3464 (19)	0.4581 (4)	0.2138 (6)	0.0169 (7)*
O5	0.062 (2)	0.6541 (4)	0.1459 (6)	0.0125 (7)*
O6	0.1767 (18)	0.3842 (4)	0.6242 (6)	0.0137 (7)*
O7	0.1543 (18)	0.0981 (4)	0.2161 (6)	0.0172 (7)*
O8	0.1706 (18)	0.1186 (4)	0.8111 (6)	0.0166 (7)*
O9	0.3374 (18)	0.6785 (4)	0.9614 (6)	0.0164 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
?	?	?	?	?	?	?

Geometric parameters (Å, º)

Ca—B2	2.981 (17)	B3—O6	1.477 (15)
Ca—B2^i	2.927 (12)	B3—O8	1.440 (10)
Ca—B3^ii	2.973 (5)	O1—O2	2.389 (5)
Ca—O3^ii	2.411 (7)	O1—O3	2.407 (16)
Ca—O4	2.371 (12)	O1—O4	2.440 (5)
Ca—O5	2.415 (5)	O1—O5	2.460 (15)
Ca—O5^i	2.452 (4)	O1—O6^v	2.742 (16)
Ca—O6	2.415 (4)	O1—O9^iv	2.401 (5)
Ca—O6^ii	2.487 (7)	O2—O2^vi	2.914 (9)
Ca—O7	2.389 (5)	O2—O3	2.364 (14)
Ca—O9^ii	2.395 (10)	O2—O7^v	2.593 (15)
B1—B2	2.446 (9)	O2—O8^iii	2.748 (12)
B1—B3^ii	2.47 (2)	O2—O9	2.820 (8)
B1—O1	1.390 (16)	O3—O5	2.413 (6)
B1—O2	1.421 (11)	O3—O6^ii	2.350 (13)
B1—O3	1.33 (2)	O3—O7^ii	2.930 (13)
B1—O5	2.742 (12)	O3—O8^ii	2.413 (10)
B1—O7^iii	2.928 (7)	O4—O5	2.322 (13)
B2—B3^ii	2.62 (3)	O4—O9^iv	2.391 (6)
B2—O1	1.467 (12)	O4—O9^v	2.734 (14)
B2—O3	2.838 (16)	O5—O6^ii	2.398 (15)
B2—O4	1.465 (7)	O5—O8^ii	2.369 (12)
B2—O5	1.46 (3)	O5—O9^iv	2.368 (16)
B2—O9^iv	1.477 (13)	O6—O8	2.461 (5)
B3—O1^ii	2.96 (2)	O7—O8^iv	2.621 (7)
B3—O3^ii	1.491 (13)	O7—O8^vii	2.784 (13)
B3—O5^ii	1.476 (16)
B2—Ca—B2^i	102.0 (3)	O7^v—O2—O9	102.1 (3)
B2—Ca—B3^ii	52.3 (5)	O8^iii—O2—O9	83.7 (3)
B2—Ca—O3^ii	146.2 (2)	Ca^ii—O3—B1	124.8 (4)
B2—Ca—O4	29.0 (3)	Ca^ii—O3—B2	122.2 (2)
B2—Ca—O5	29.2 (5)	Ca^ii—O3—B3^ii	98.4 (7)
B2—Ca—O5^i	83.8 (3)	Ca^ii—O3—O1	130.2 (3)
B2—Ca—O6	88.2 (3)	Ca^ii—O3—O2	108.4 (2)
B2—Ca—O6^ii	81.5 (4)	Ca^ii—O3—O5	113.3 (3)
B2—Ca—O7	113.4 (4)	Ca^ii—O3—O6^ii	60.9 (3)
B2—Ca—O9^ii	127.8 (3)	Ca^ii—O3—O7^ii	52.0 (2)
B2^i—Ca—B3^ii	94.7 (2)	Ca^ii—O3—O8^ii	114.2 (5)
B2^i—Ca—O3^ii	110.3 (4)	B1—O3—B2	59.4 (5)
B2^i—Ca—O4	112.2 (4)	B1—O3—B3^ii	122.7 (8)
B2^i—Ca—O5	85.6 (2)	B1—O3—O1	28.3 (3)
B2^i—Ca—O5^i	30.0 (5)	B1—O3—O2	31.8 (4)
B2^i—Ca—O6	165.0 (5)	B1—O3—O5	89.4 (6)
B2^i—Ca—O6^ii	94.3 (3)	B1—O3—O6^ii	144.2 (5)
B2^i—Ca—O7	93.6 (2)	B1—O3—O7^ii	132.1 (4)
B2^i—Ca—O9^ii	30.2 (4)	B1—O3—O8^ii	120.5 (5)
B3^ii—Ca—O3^ii	113.4 (3)	B2—O3—B3^ii	66.4 (8)
B3^ii—Ca—O4	79.8 (4)	B2—O3—O1	31.1 (4)
B3^ii—Ca—O5	29.5 (4)	B2—O3—O2	91.2 (6)
B3^ii—Ca—O5^i	102.17 (14)	B2—O3—O5	31.1 (5)
B3^ii—Ca—O6	82.67 (16)	B2—O3—O6^ii	87.0 (4)
B3^ii—Ca—O6^ii	29.7 (4)	B2—O3—O7^ii	168.3 (6)
B3^ii—Ca—O7	164.8 (5)	B2—O3—O8^ii	84.1 (4)
B3^ii—Ca—O9^ii	98.8 (3)	B3^ii—O3—O1	95.7 (7)
O3^ii—Ca—O4	134.0 (3)	B3^ii—O3—O2	151.8 (8)
O3^ii—Ca—O5	142.7 (2)	B3^ii—O3—O5	35.3 (7)
O3^ii—Ca—O5^i	129.8 (3)	B3^ii—O3—O6^ii	37.5 (5)
O3^ii—Ca—O6	58.3 (3)	B3^ii—O3—O7^ii	103.3 (9)
O3^ii—Ca—O6^ii	85.9 (2)	B3^ii—O3—O8^ii	33.9 (3)
O3^ii—Ca—O7	75.2 (3)	O1—O3—O2	60.1 (4)
O3^ii—Ca—O9^ii	81.4 (3)	O1—O3—O5	61.4 (4)
O4—Ca—O5	58.0 (3)	O1—O3—O6^ii	117.5 (3)
O4—Ca—O5^i	84.8 (3)	O1—O3—O7^ii	160.4 (4)
O4—Ca—O6	82.0 (3)	O1—O3—O8^ii	103.8 (3)
O4—Ca—O6^ii	107.3 (3)	O2—O3—O5	121.1 (6)
O4—Ca—O7	85.3 (3)	O2—O3—O6^ii	165.2 (3)
O4—Ca—O9^ii	142.4 (2)	O2—O3—O7^ii	100.3 (3)
O5—Ca—O5^i	80.31 (14)	O2—O3—O8^ii	132.3 (3)
O5—Ca—O6	98.67 (16)	O5—O3—O6^ii	60.5 (4)
O5—Ca—O6^ii	58.6 (3)	O5—O3—O7^ii	138.1 (6)
O5—Ca—O7	139.3 (4)	O5—O3—O8^ii	58.8 (3)
O5—Ca—O9^ii	103.8 (3)	O6^ii—O3—O7^ii	81.3 (4)
O5^i—Ca—O6	164.9 (4)	O6^ii—O3—O8^ii	62.2 (3)
O5^i—Ca—O6^ii	115.2 (2)	O7^ii—O3—O8^ii	89.6 (4)
O5^i—Ca—O7	79.19 (16)	Ca—O4—B2	99.3 (11)
O5^i—Ca—O9^ii	58.5 (4)	Ca—O4—O1	112.9 (5)
O6—Ca—O6^ii	76.0 (2)	Ca—O4—O5	61.9 (4)
O6—Ca—O7	92.44 (17)	Ca—O4—O9^iv	115.4 (5)
O6—Ca—O9^ii	135.5 (3)	Ca—O4—O9^v	134.5 (2)
O6^ii—Ca—O7	161.1 (2)	B2—O4—O1	33.7 (5)
O6^ii—Ca—O9^ii	83.7 (3)	B2—O4—O5	37.6 (10)
O7—Ca—O9^ii	94.8 (3)	B2—O4—O9^iv	35.8 (5)
B2—B1—B3^ii	64.5 (6)	B2—O4—O9^v	116.0 (9)
B2—B1—O1	32.1 (7)	O1—O4—O5	62.2 (3)
B2—B1—O2	148.3 (14)	O1—O4—O9^iv	59.59 (16)
B2—B1—O3	92.8 (7)	O1—O4—O9^v	112.4 (5)
B2—B1—O5	32.2 (6)	O5—O4—O9^iv	60.3 (4)
B2—B1—O7^iii	90.2 (3)	O5—O4—O9^v	142.1 (3)
B3^ii—B1—O1	95.7 (7)	O9^iv—O4—O9^v	84.1 (4)
B3^ii—B1—O2	146.9 (11)	Ca—O5—Ca^i	99.69 (15)
B3^ii—B1—O3	30.5 (4)	Ca—O5—B1	109.4 (2)
B3^ii—B1—O5	32.3 (4)	Ca—O5—B2	97.4 (4)
B3^ii—B1—O7^iii	76.1 (4)	Ca—O5—B3^ii	96.7 (5)
O1—B1—O2	116.4 (14)	Ca—O5—O1	110.6 (3)
O1—B1—O3	124.8 (8)	Ca—O5—O3	100.4 (2)
O1—B1—O5	63.5 (6)	Ca—O5—O4	60.0 (3)
O1—B1—O7^iii	91.0 (4)	Ca—O5—O6^ii	62.2 (2)
O2—B1—O3	118.8 (10)	Ca—O5—O8^ii	122.5 (6)
O2—B1—O5	175.4 (4)	Ca—O5—O9^iv	114.6 (4)
O2—B1—O7^iii	94.6 (3)	Ca^i—O5—B1	143.8 (5)
O3—B1—O5	61.6 (5)	Ca^i—O5—B2	93.3 (5)
O3—B1—O7^iii	86.1 (6)	Ca^i—O5—B3^ii	134.5 (7)
O5—B1—O7^iii	80.8 (3)	Ca^i—O5—O1	118.7 (5)
Ca—B2—Ca^i	78.0 (4)	Ca^i—O5—O3	158.87 (17)
Ca—B2—B1	101.4 (6)	Ca^i—O5—O4	94.8 (3)
Ca—B2—B3^ii	63.7 (5)	Ca^i—O5—O6^ii	127.6 (5)
Ca—B2—O1	125.1 (7)	Ca^i—O5—O8^ii	102.5 (3)
Ca—B2—O3	79.2 (5)	Ca^i—O5—O9^iv	59.5 (2)
Ca—B2—O4	51.7 (8)	B1—O5—B2	62.7 (5)
Ca—B2—O5	53.5 (5)	B1—O5—B3^ii	63.8 (7)
Ca—B2—O9^iv	125.6 (6)	B1—O5—O1	30.4 (4)
Ca^i—B2—B1	133.4 (8)	B1—O5—O3	28.9 (5)
Ca^i—B2—B3^ii	81.8 (6)	B1—O5—O4	82.2 (4)
Ca^i—B2—O1	146.3 (4)	B1—O5—O6^ii	85.9 (4)
Ca^i—B2—O3	112.1 (7)	B1—O5—O8^ii	79.8 (4)
Ca^i—B2—O4	101.0 (5)	B1—O5—O9^iv	88.4 (5)
Ca^i—B2—O5	56.8 (4)	B2—O5—B3^ii	126.4 (8)
Ca^i—B2—O9^iv	54.6 (6)	B2—O5—O1	33.0 (3)
B1—B2—B3^ii	58.3 (6)	B2—O5—O3	90.7 (5)
B1—B2—O1	30.2 (7)	B2—O5—O4	37.6 (4)
B1—B2—O3	27.8 (5)	B2—O5—O6^ii	135.2 (4)
B1—B2—O4	115.2 (4)	B2—O5—O8^ii	132.9 (5)
B1—B2—O5	85.1 (8)	B2—O5—O9^iv	36.6 (4)
B1—B2—O9^iv	129.4 (6)	B3^ii—O5—O1	94.0 (7)
B3^ii—B2—O1	87.8 (8)	B3^ii—O5—O3	35.8 (6)
B3^ii—B2—O3	31.4 (3)	B3^ii—O5—O4	129.9 (4)
B3^ii—B2—O4	112.4 (11)	B3^ii—O5—O6^ii	35.7 (5)
B3^ii—B2—O5	26.9 (4)	B3^ii—O5—O8^ii	35.2 (3)
B3^ii—B2—O9^iv	124.4 (9)	B3^ii—O5—O9^iv	144.1 (6)
O1—B2—O3	58.0 (7)	O1—O5—O3	59.2 (4)
O1—B2—O4	112.6 (9)	O1—O5—O4	61.3 (4)
O1—B2—O5	114.1 (10)	O1—O5—O6^ii	113.6 (3)
O1—B2—O9^iv	109.2 (11)	O1—O5—O8^ii	103.6 (3)
O3—B2—O4	112.2 (7)	O1—O5—O9^iv	59.6 (4)
O3—B2—O5	58.2 (5)	O3—O5—O4	101.0 (4)
O3—B2—O9^iv	138.9 (5)	O3—O5—O6^ii	58.5 (3)
O4—B2—O5	104.8 (11)	O3—O5—O8^ii	60.6 (3)
O4—B2—O9^iv	108.7 (8)	O3—O5—O9^iv	116.7 (5)
O5—B2—O9^iv	107.2 (9)	O4—O5—O6^ii	112.0 (3)
Ca^ii—B3—B1^ii	101.0 (5)	O4—O5—O8^ii	161.4 (3)
Ca^ii—B3—B2^ii	64.0 (3)	O4—O5—O9^iv	61.3 (4)
Ca^ii—B3—O1^ii	85.1 (4)	O6^ii—O5—O8^ii	62.2 (4)
Ca^ii—B3—O3^ii	107.7 (5)	O6^ii—O5—O9^iv	171.8 (4)
Ca^ii—B3—O5^ii	53.8 (3)	O8^ii—O5—O9^iv	122.5 (3)
Ca^ii—B3—O6	56.6 (3)	Ca—O6—Ca^ii	104.0 (3)
Ca^ii—B3—O8	141.3 (5)	Ca—O6—B3	98.6 (5)
B1^ii—B3—B2^ii	57.3 (5)	Ca—O6—O1^v	105.6 (3)
B1^ii—B3—O1^ii	27.9 (4)	Ca—O6—O3^ii	60.8 (2)
B1^ii—B3—O3^ii	26.8 (6)	Ca—O6—O5^ii	113.7 (5)
B1^ii—B3—O5^ii	83.9 (9)	Ca—O6—O8	112.3 (2)
B1^ii—B3—O6	123.5 (5)	Ca^ii—O6—B3	93.7 (6)
B1^ii—B3—O8	111.7 (7)	Ca^ii—O6—O1^v	137.9 (3)
B2^ii—B3—O1^ii	29.7 (3)	Ca^ii—O6—O3^ii	100.1 (5)
B2^ii—B3—O3^ii	82.3 (9)	Ca^ii—O6—O5^ii	59.2 (2)
B2^ii—B3—O5^ii	26.7 (6)	Ca^ii—O6—O8	115.9 (4)
B2^ii—B3—O6	119.5 (6)	B3—O6—O1^v	110.6 (6)
B2^ii—B3—O8	117.8 (8)	B3—O6—O3^ii	37.9 (4)
O1^ii—B3—O3^ii	54.1 (7)	B3—O6—O5^ii	35.7 (4)
O1^ii—B3—O5^ii	56.1 (7)	B3—O6—O8	32.0 (6)
O1^ii—B3—O6	130.0 (6)	O1^v—O6—O3^ii	120.3 (3)
O1^ii—B3—O8	114.9 (8)	O1^v—O6—O5^ii	129.9 (3)
O3^ii—B3—O5^ii	108.9 (13)	O1^v—O6—O8	78.9 (3)
O3^ii—B3—O6	104.7 (5)	O3^ii—O6—O5^ii	61.1 (3)
O3^ii—B3—O8	110.8 (4)	O3^ii—O6—O8	60.2 (3)
O5^ii—B3—O6	108.6 (5)	O5^ii—O6—O8	58.3 (3)
O5^ii—B3—O8	108.7 (6)	Ca—O7—B1^viii	139.0 (3)
O6—B3—O8	115.0 (13)	Ca—O7—O2^v	107.4 (3)
B1—O1—B2	117.7 (13)	Ca—O7—O3^ii	52.71 (18)
B1—O1—B3^ii	56.4 (8)	Ca—O7—O8^iv	97.18 (16)
B1—O1—O2	32.2 (7)	Ca—O7—O8^vii	108.1 (4)
B1—O1—O3	26.9 (7)	B1^viii—O7—O2^v	71.6 (4)
B1—O1—O4	119.1 (7)	B1^viii—O7—O3^ii	90.8 (3)
B1—O1—O5	86.1 (9)	B1^viii—O7—O8^iv	123.7 (3)
B1—O1—O6^v	131.2 (7)	B1^viii—O7—O8^vii	70.3 (4)
B1—O1—O9^iv	139.3 (9)	O2^v—O7—O3^ii	119.0 (3)
B2—O1—B3^ii	62.5 (9)	O2^v—O7—O8^iv	91.7 (4)
B2—O1—O2	149.8 (11)	O2^v—O7—O8^vii	140.4 (2)
B2—O1—O3	90.9 (10)	O3^ii—O7—O8^iv	140.8 (4)
B2—O1—O4	33.7 (4)	O3^ii—O7—O8^vii	71.9 (3)
B2—O1—O5	32.9 (9)	O8^iv—O7—O8^vii	100.6 (3)
B2—O1—O6^v	102.5 (9)	B3—O8—O2^viii	128.6 (6)
B2—O1—O9^iv	35.5 (6)	B3—O8—O3^ii	35.3 (4)
B3^ii—O1—O2	88.3 (4)	B3—O8—O5^ii	36.2 (5)
B3^ii—O1—O3	30.1 (2)	B3—O8—O6	33.0 (8)
B3^ii—O1—O4	79.1 (4)	B3—O8—O7^ix	112.3 (6)
B3^ii—O1—O5	29.9 (3)	B3—O8—O7^vii	99.9 (8)
B3^ii—O1—O6^v	158.2 (2)	O2^viii—O8—O3^ii	107.5 (3)
B3^ii—O1—O9^iv	85.7 (4)	O2^viii—O8—O5^ii	164.7 (3)
O2—O1—O3	59.1 (4)	O2^viii—O8—O6	106.5 (4)
O2—O1—O4	138.8 (3)	O2^viii—O8—O7^ix	118.8 (3)
O2—O1—O5	118.2 (6)	O2^viii—O8—O7^vii	95.1 (3)
O2—O1—O6^v	103.0 (4)	O3^ii—O8—O5^ii	60.6 (3)
O2—O1—O9^iv	159.1 (2)	O3^ii—O8—O6	57.6 (3)
O3—O1—O4	97.8 (5)	O3^ii—O8—O7^ix	127.9 (6)
O3—O1—O5	59.4 (4)	O3^ii—O8—O7^vii	73.7 (4)
O3—O1—O6^v	149.7 (2)	O5^ii—O8—O6	59.5 (3)
O3—O1—O9^iv	115.6 (5)	O5^ii—O8—O7^ix	76.2 (3)
O4—O1—O5	56.6 (3)	O5^ii—O8—O7^vii	90.7 (5)
O4—O1—O6^v	80.2 (4)	O6—O8—O7^ix	123.01 (19)
O4—O1—O9^iv	59.19 (16)	O6—O8—O7^vii	130.5 (4)
O5—O1—O6^v	134.6 (3)	O7^ix—O8—O7^vii	79.4 (3)
O5—O1—O9^iv	58.3 (4)	Ca^ii—O9—B2^ix	95.3 (10)
O6^v—O1—O9^iv	89.5 (4)	Ca^ii—O9—O1^ix	123.7 (5)
B1—O2—O1	31.4 (8)	Ca^ii—O9—O2	95.6 (2)
B1—O2—O2^vi	89.9 (5)	Ca^ii—O9—O4^ix	94.5 (4)
B1—O2—O3	29.5 (8)	Ca^ii—O9—O4^v	112.7 (2)
B1—O2—O7^v	129.6 (9)	Ca^ii—O9—O5^ix	62.0 (3)
B1—O2—O8^iii	108.3 (9)	B2^ix—O9—O1^ix	35.2 (6)
B1—O2—O9	89.5 (5)	B2^ix—O9—O2	154.2 (3)
O1—O2—O2^vi	71.8 (2)	B2^ix—O9—O4^ix	35.5 (4)
O1—O2—O3	60.9 (4)	B2^ix—O9—O4^v	127.0 (8)
O1—O2—O7^v	99.2 (5)	B2^ix—O9—O5^ix	36.2 (9)
O1—O2—O8^iii	135.6 (5)	O1^ix—O9—O2	121.5 (3)
O1—O2—O9	105.7 (2)	O1^ix—O9—O4^ix	61.22 (16)
O2^vi—O2—O3	107.6 (2)	O1^ix—O9—O4^v	119.3 (5)
O2^vi—O2—O7^v	74.8 (3)	O1^ix—O9—O5^ix	62.1 (4)
O2^vi—O2—O8^iii	100.7 (2)	O2—O9—O4^ix	164.2 (6)
O2^vi—O2—O9	175.5 (4)	O2—O9—O4^v	68.9 (3)
O3—O2—O7^v	156.2 (3)	O2—O9—O5^ix	137.4 (4)
O3—O2—O8^iii	81.8 (4)	O4^ix—O9—O4^v	95.9 (3)
O3—O2—O9	73.8 (3)	O4^ix—O9—O5^ix	58.4 (3)
O7^v—O2—O8^iii	121.5 (3)	O4^v—O9—O5^ix	151.3 (2)

Symmetry codes: (i) −x, −y+1, −z; (ii) −x, −y+1, −z+1; (iii) x, y+1, z; (iv) x, y, z−1; (v) −x+1, −y+1, −z+1; (vi) −x+1, −y+2, −z+1; (vii) −x, −y, −z+1; (viii) x, y−1, z; (ix) x, y, z+1.

(I_3.14GPa)

Crystal data

H7B3CaO9	Z = 2
Mr = 223.6	F(000) = 214
Triclinic, P1	Dx = 2.224 Mg m^−3
Hall symbol: -P 1	Synchrotron radiation, λ = 0.41066 Å
a = 6.465 (3) Å	Cell parameters from 718 reflections
b = 8.059 (3) Å	θ = 2.4–19.6°
c = 6.388 (3) Å	µ = 0.22 mm^−1
α = 89.922 (3)°	T = 293 K
β = 103.38 (1)°	Prismatic habit, colourless
γ = 86.859 (10)°	0.02 × 0.01 × 0.01 mm
V = 323.3 (2) Å^3

Data collection

Beamline diffractometer	437 reflections with I > 3σ(I)
Radiation source: ESRF: Synchrotron radiation, undulator, IVU20c	Rint = 0.013
Silicon monochromator	θmax = 19.6°, θmin = 2.3°
ω scans	h = −4→2
718 measured reflections	k = −12→12
479 independent reflections	l = −9→9

Refinement

Refinement on F	0 constraints
R[F^2 > 2σ(F^2)] = 0.047	H-atom parameters not defined
wR(F^2) = 0.063	Weighting scheme based on measured s.u.'s w = 1/(σ^2(F) + 0.0001F^2)
S = 3.48	(Δ/σ)max = 0.015
479 reflections	Δρmax = 0.33 e Å^−3
53 parameters	Δρmin = −0.27 e Å^−3
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ca	0.0100 (5)	0.37346 (11)	0.24576 (17)	0.0125 (3)*
B1	0.310 (3)	0.8070 (7)	0.4896 (11)	0.0135 (10)*
B2	0.295 (4)	0.6347 (7)	0.1720 (11)	0.0137 (11)*
B3	0.053 (3)	0.2623 (6)	0.7058 (10)	0.0139 (10)*
O1	0.411 (2)	0.7404 (4)	0.3383 (7)	0.0179 (8)*
O2	0.4387 (18)	0.8965 (4)	0.6594 (6)	0.0154 (7)*
O3	0.111 (2)	0.7868 (4)	0.4910 (7)	0.0141 (7)*
O4	0.346 (2)	0.4576 (4)	0.2144 (7)	0.0179 (8)*
O5	0.061 (2)	0.6539 (4)	0.1465 (7)	0.0131 (8)*
O6	0.1791 (19)	0.3841 (4)	0.6245 (6)	0.0142 (7)*
O7	0.153 (2)	0.0979 (4)	0.2161 (6)	0.0172 (8)*
O8	0.170 (2)	0.1184 (4)	0.8114 (7)	0.0175 (8)*
O9	0.3386 (19)	0.6788 (4)	0.9620 (6)	0.0165 (8)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
?	?	?	?	?	?	?

Geometric parameters (Å, º)

Ca—B2	2.977 (17)	B3—O6	1.475 (16)
Ca—B2^i	2.930 (13)	B3—O8	1.427 (10)
Ca—B3^ii	2.968 (6)	O1—O2	2.384 (6)
Ca—O3^ii	2.414 (8)	O1—O3	2.378 (17)
Ca—O4	2.364 (13)	O1—O4	2.440 (6)
Ca—O5	2.407 (5)	O1—O5	2.451 (16)
Ca—O5^i	2.453 (5)	O1—O6^v	2.737 (17)
Ca—O6	2.417 (5)	O1—O9^iv	2.398 (6)
Ca—O6^ii	2.492 (7)	O2—O2^vi	2.906 (9)
Ca—O7	2.383 (6)	O2—O3	2.361 (15)
Ca—O9^ii	2.395 (11)	O2—O7^v	2.578 (17)
B1—B2	2.446 (10)	O2—O8^iii	2.756 (12)
B1—B3^ii	2.49 (2)	O2—O9	2.815 (9)
B1—O1	1.380 (16)	O3—O5	2.410 (6)
B1—O2	1.427 (12)	O3—O6^ii	2.368 (14)
B1—O3	1.31 (2)	O3—O7^ii	2.931 (14)
B1—O5	2.741 (12)	O3—O8^ii	2.417 (11)
B1—O7^iii	2.914 (8)	O4—O5	2.323 (14)
B2—B3^ii	2.64 (3)	O4—O9^iv	2.393 (6)
B2—O1	1.458 (12)	O4—O9^v	2.730 (15)
B2—O3	2.833 (17)	O5—O6^ii	2.397 (16)
B2—O4	1.458 (7)	O5—O8^ii	2.359 (13)
B2—O5	1.48 (3)	O5—O9^iv	2.380 (17)
B2—O9^iv	1.481 (14)	O6—O8	2.459 (6)
B3—O1^ii	2.95 (2)	O7—O8^iv	2.619 (8)
B3—O3^ii	1.515 (14)	O7—O8^vii	2.769 (14)
B3—O5^ii	1.471 (17)
B2—Ca—B2^i	102.1 (4)	O7^v—O2—O9	102.5 (3)
B2—Ca—B3^ii	52.7 (5)	O8^iii—O2—O9	83.4 (3)
B2—Ca—O3^ii	146.2 (2)	Ca^ii—O3—B1	125.5 (5)
B2—Ca—O4	28.9 (4)	Ca^ii—O3—B2	122.1 (2)
B2—Ca—O5	29.6 (5)	Ca^ii—O3—B3^ii	97.7 (7)
B2—Ca—O5^i	83.7 (3)	Ca^ii—O3—O1	130.5 (3)
B2—Ca—O6	87.7 (3)	Ca^ii—O3—O2	108.5 (2)
B2—Ca—O6^ii	81.9 (4)	Ca^ii—O3—O5	112.9 (3)
B2—Ca—O7	113.4 (4)	Ca^ii—O3—O6^ii	60.7 (3)
B2—Ca—O9^ii	128.0 (3)	Ca^ii—O3—O7^ii	51.9 (2)
B2^i—Ca—B3^ii	94.3 (2)	Ca^ii—O3—O8^ii	113.7 (6)
B2^i—Ca—O3^ii	110.1 (4)	B1—O3—B2	59.6 (6)
B2^i—Ca—O4	112.2 (4)	B1—O3—B3^ii	123.3 (9)
B2^i—Ca—O5	85.5 (3)	B1—O3—O1	28.6 (4)
B2^i—Ca—O5^i	30.3 (5)	B1—O3—O2	31.8 (4)
B2^i—Ca—O6	165.3 (5)	B1—O3—O5	89.9 (6)
B2^i—Ca—O6^ii	94.1 (3)	B1—O3—O6^ii	144.8 (5)
B2^i—Ca—O7	93.6 (2)	B1—O3—O7^ii	132.2 (4)
B2^i—Ca—O9^ii	30.2 (4)	B1—O3—O8^ii	120.3 (5)
B3^ii—Ca—O3^ii	113.2 (3)	B2—O3—B3^ii	67.0 (8)
B3^ii—Ca—O4	80.2 (4)	B2—O3—O1	31.0 (4)
B3^ii—Ca—O5	29.5 (4)	B2—O3—O2	91.3 (6)
B3^ii—Ca—O5^i	102.04 (15)	B2—O3—O5	31.5 (5)
B3^ii—Ca—O6	82.89 (17)	B2—O3—O6^ii	87.2 (4)
B3^ii—Ca—O6^ii	29.7 (4)	B2—O3—O7^ii	168.1 (6)
B3^ii—Ca—O7	165.4 (5)	B2—O3—O8^ii	84.3 (4)
B3^ii—Ca—O9^ii	98.5 (3)	B3^ii—O3—O1	96.1 (8)
O3^ii—Ca—O4	134.2 (3)	B3^ii—O3—O2	152.5 (8)
O3^ii—Ca—O5	142.4 (2)	B3^ii—O3—O5	35.6 (7)
O3^ii—Ca—O5^i	129.9 (3)	B3^ii—O3—O6^ii	37.0 (5)
O3^ii—Ca—O6	58.7 (3)	B3^ii—O3—O7^ii	102.5 (9)
O3^ii—Ca—O6^ii	85.6 (2)	B3^ii—O3—O8^ii	33.6 (3)
O3^ii—Ca—O7	75.3 (3)	O1—O3—O2	60.4 (4)
O3^ii—Ca—O9^ii	81.1 (3)	O1—O3—O5	61.6 (4)
O4—Ca—O5	58.3 (4)	O1—O3—O6^ii	117.6 (3)
O4—Ca—O5^i	84.6 (3)	O1—O3—O7^ii	160.8 (4)
O4—Ca—O6	81.6 (3)	O1—O3—O8^ii	103.7 (4)
O4—Ca—O6^ii	107.6 (3)	O2—O3—O5	121.7 (6)
O4—Ca—O7	85.4 (3)	O2—O3—O6^ii	165.3 (3)
O4—Ca—O9^ii	142.5 (2)	O2—O3—O7^ii	100.3 (3)
O5—Ca—O5^i	80.30 (15)	O2—O3—O8^ii	132.5 (3)
O5—Ca—O6	98.50 (18)	O5—O3—O6^ii	60.2 (4)
O5—Ca—O6^ii	58.6 (3)	O5—O3—O7^ii	137.5 (6)
O5—Ca—O7	139.6 (4)	O5—O3—O8^ii	58.5 (3)
O5—Ca—O9^ii	103.8 (3)	O6^ii—O3—O7^ii	80.9 (5)
O5^i—Ca—O6	164.3 (5)	O6^ii—O3—O8^ii	61.8 (3)
O5^i—Ca—O6^ii	115.2 (2)	O7^ii—O3—O8^ii	89.5 (5)
O5^i—Ca—O7	79.07 (17)	Ca—O4—B2	99.6 (11)
O5^i—Ca—O9^ii	58.8 (4)	Ca—O4—O1	112.6 (5)
O6—Ca—O6^ii	76.3 (2)	Ca—O4—O5	61.8 (4)
O6—Ca—O7	92.43 (18)	Ca—O4—O9^iv	115.6 (5)
O6—Ca—O9^ii	135.8 (4)	Ca—O4—O9^v	134.4 (2)
O6^ii—Ca—O7	160.9 (3)	B2—O4—O1	33.2 (5)
O6^ii—Ca—O9^ii	83.5 (3)	B2—O4—O5	38.1 (10)
O7—Ca—O9^ii	94.6 (3)	B2—O4—O9^iv	35.8 (6)
B2—B1—B3^ii	64.7 (7)	B2—O4—O9^v	115.7 (10)
B2—B1—O1	31.4 (7)	O1—O4—O5	61.9 (4)
B2—B1—O2	147.5 (14)	O1—O4—O9^iv	59.48 (17)
B2—B1—O3	93.0 (8)	O1—O4—O9^v	112.8 (5)
B2—B1—O5	32.5 (6)	O5—O4—O9^iv	60.6 (4)
B2—B1—O7^iii	90.5 (3)	O5—O4—O9^v	142.0 (3)
B3^ii—B1—O1	95.3 (7)	O9^iv—O4—O9^v	83.8 (4)
B3^ii—B1—O2	147.6 (11)	Ca—O5—Ca^i	99.70 (16)
B3^ii—B1—O3	30.6 (4)	Ca—O5—B1	109.7 (2)
B3^ii—B1—O5	32.2 (4)	Ca—O5—B2	97.1 (4)
B3^ii—B1—O7^iii	76.0 (4)	Ca—O5—B3^ii	96.9 (6)
O1—B1—O2	116.3 (15)	Ca—O5—O1	110.7 (3)
O1—B1—O3	124.4 (9)	Ca—O5—O3	100.7 (2)
O1—B1—O5	63.2 (6)	Ca—O5—O4	59.9 (3)
O1—B1—O7^iii	91.2 (4)	Ca—O5—O6^ii	62.5 (3)
O2—B1—O3	119.3 (10)	Ca—O5—O8^ii	123.0 (6)
O2—B1—O5	176.2 (4)	Ca—O5—O9^iv	114.4 (4)
O2—B1—O7^iii	95.4 (3)	Ca^i—O5—B1	143.3 (6)
O3—B1—O5	61.6 (5)	Ca^i—O5—B2	93.0 (5)
O3—B1—O7^iii	86.4 (6)	Ca^i—O5—B3^ii	134.1 (7)
O5—B1—O7^iii	80.9 (3)	Ca^i—O5—O1	118.5 (5)
Ca—B2—Ca^i	77.9 (4)	Ca^i—O5—O3	158.80 (18)
Ca—B2—B1	101.6 (7)	Ca^i—O5—O4	94.5 (3)
Ca—B2—B3^ii	63.5 (5)	Ca^i—O5—O6^ii	127.8 (6)
Ca—B2—O1	125.0 (7)	Ca^i—O5—O8^ii	102.6 (3)
Ca—B2—O3	79.3 (5)	Ca^i—O5—O9^iv	59.4 (3)
Ca—B2—O4	51.5 (8)	B1—O5—B2	62.7 (5)
Ca—B2—O5	53.4 (5)	B1—O5—B3^ii	64.3 (7)
Ca—B2—O9^iv	125.7 (6)	B1—O5—O1	30.2 (4)
Ca^i—B2—B1	132.8 (8)	B1—O5—O3	28.5 (5)
Ca^i—B2—B3^ii	81.3 (6)	B1—O5—O4	82.3 (5)
Ca^i—B2—O1	145.6 (4)	B1—O5—O6^ii	86.2 (4)
Ca^i—B2—O3	112.1 (7)	B1—O5—O8^ii	79.6 (4)
Ca^i—B2—O4	100.8 (5)	B1—O5—O9^iv	88.0 (6)
Ca^i—B2—O5	56.7 (4)	B2—O5—B3^ii	126.9 (8)
Ca^i—B2—O9^iv	54.5 (6)	B2—O5—O1	33.2 (4)
B1—B2—B3^ii	58.4 (6)	B2—O5—O3	90.2 (5)
B1—B2—O1	29.6 (7)	B2—O5—O4	37.4 (4)
B1—B2—O3	27.5 (5)	B2—O5—O6^ii	135.3 (4)
B1—B2—O4	115.7 (4)	B2—O5—O8^ii	132.8 (5)
B1—B2—O5	84.8 (8)	B2—O5—O9^iv	36.5 (4)
B1—B2—O9^iv	129.0 (6)	B3^ii—O5—O1	94.4 (7)
B3^ii—B2—O1	87.2 (9)	B3^ii—O5—O3	36.8 (7)
B3^ii—B2—O3	31.9 (4)	B3^ii—O5—O4	130.5 (5)
B3^ii—B2—O4	112.2 (11)	B3^ii—O5—O6^ii	35.6 (5)
B3^ii—B2—O5	26.5 (4)	B3^ii—O5—O8^ii	34.9 (3)
B3^ii—B2—O9^iv	123.8 (9)	B3^ii—O5—O9^iv	144.2 (7)
O1—B2—O3	57.0 (7)	O1—O5—O3	58.6 (4)
O1—B2—O4	113.6 (9)	O1—O5—O4	61.4 (4)
O1—B2—O5	113.1 (11)	O1—O5—O6^ii	113.7 (3)
O1—B2—O9^iv	109.3 (12)	O1—O5—O8^ii	103.2 (3)
O3—B2—O4	112.3 (7)	O1—O5—O9^iv	59.5 (4)
O3—B2—O5	58.3 (6)	O3—O5—O4	100.7 (4)
O3—B2—O9^iv	138.5 (5)	O3—O5—O6^ii	59.0 (4)
O4—B2—O5	104.5 (12)	O3—O5—O8^ii	60.9 (3)
O4—B2—O9^iv	109.0 (9)	O3—O5—O9^iv	116.0 (6)
O5—B2—O9^iv	107.0 (9)	O4—O5—O6^ii	112.3 (3)
Ca^ii—B3—B1^ii	100.8 (5)	O4—O5—O8^ii	161.4 (3)
Ca^ii—B3—B2^ii	63.8 (3)	O4—O5—O9^iv	61.1 (4)
Ca^ii—B3—O1^ii	84.9 (4)	O6^ii—O5—O8^ii	62.3 (4)
Ca^ii—B3—O3^ii	107.1 (5)	O6^ii—O5—O9^iv	171.8 (5)
Ca^ii—B3—O5^ii	53.6 (3)	O8^ii—O5—O9^iv	122.2 (3)
Ca^ii—B3—O6	56.9 (4)	Ca—O6—Ca^ii	103.7 (3)
Ca^ii—B3—O8	142.1 (6)	Ca—O6—B3	98.7 (5)
B1^ii—B3—B2^ii	56.9 (6)	Ca—O6—O1^v	105.7 (3)
B1^ii—B3—O1^ii	27.7 (4)	Ca—O6—O3^ii	60.6 (2)
B1^ii—B3—O3^ii	26.1 (7)	Ca—O6—O5^ii	113.3 (5)
B1^ii—B3—O5^ii	83.5 (10)	Ca—O6—O8	112.1 (2)
B1^ii—B3—O6	123.3 (6)	Ca^ii—O6—B3	93.3 (7)
B1^ii—B3—O8	110.8 (7)	Ca^ii—O6—O1^v	138.3 (3)
B2^ii—B3—O1^ii	29.5 (3)	Ca^ii—O6—O3^ii	99.5 (5)
B2^ii—B3—O3^ii	81.1 (9)	Ca^ii—O6—O5^ii	59.0 (2)
B2^ii—B3—O5^ii	26.6 (6)	Ca^ii—O6—O8	115.5 (4)
B2^ii—B3—O6	119.5 (6)	B3—O6—O1^v	110.5 (7)
B2^ii—B3—O8	117.6 (9)	B3—O6—O3^ii	38.2 (4)
O1^ii—B3—O3^ii	53.2 (8)	B3—O6—O5^ii	35.5 (5)
O1^ii—B3—O5^ii	55.9 (8)	B3—O6—O8	31.5 (7)
O1^ii—B3—O6	129.8 (7)	O1^v—O6—O3^ii	120.6 (3)
O1^ii—B3—O8	114.2 (9)	O1^v—O6—O5^ii	130.1 (3)
O3^ii—B3—O5^ii	107.6 (13)	O1^v—O6—O8	79.3 (4)
O3^ii—B3—O6	104.7 (6)	O3^ii—O6—O5^ii	60.8 (4)
O3^ii—B3—O8	110.4 (5)	O3^ii—O6—O8	60.1 (3)
O5^ii—B3—O6	108.9 (5)	O5^ii—O6—O8	58.1 (3)
O5^ii—B3—O8	108.9 (6)	Ca—O7—B1^viii	139.0 (3)
O6—B3—O8	115.8 (14)	Ca—O7—O2^v	107.2 (3)
B1—O1—B2	119.0 (14)	Ca—O7—O3^ii	52.8 (2)
B1—O1—B3^ii	57.0 (8)	Ca—O7—O8^iv	97.23 (17)
B1—O1—O2	32.5 (7)	Ca—O7—O8^vii	108.4 (5)
B1—O1—O3	27.0 (8)	B1^viii—O7—O2^v	71.6 (4)
B1—O1—O4	119.7 (8)	B1^viii—O7—O3^ii	90.9 (4)
B1—O1—O5	86.6 (9)	B1^viii—O7—O8^iv	123.6 (4)
B1—O1—O6^v	131.1 (7)	B1^viii—O7—O8^vii	70.4 (4)
B1—O1—O9^iv	140.1 (9)	O2^v—O7—O3^ii	119.1 (3)
B2—O1—B3^ii	63.2 (10)	O2^v—O7—O8^iv	91.4 (5)
B2—O1—O2	151.2 (12)	O2^v—O7—O8^vii	140.4 (3)
B2—O1—O3	92.0 (11)	O3^ii—O7—O8^iv	140.9 (4)
B2—O1—O4	33.2 (4)	O3^ii—O7—O8^vii	72.0 (4)
B2—O1—O5	33.7 (9)	O8^iv—O7—O8^vii	100.6 (3)
B2—O1—O6^v	101.3 (9)	B3—O8—O2^viii	128.5 (6)
B2—O1—O9^iv	35.6 (6)	B3—O8—O3^ii	36.0 (4)
B3^ii—O1—O2	89.2 (5)	B3—O8—O5^ii	36.1 (5)
B3^ii—O1—O3	30.7 (3)	B3—O8—O6	32.7 (8)
B3^ii—O1—O4	79.3 (4)	B3—O8—O7^ix	112.2 (6)
B3^ii—O1—O5	29.8 (3)	B3—O8—O7^vii	100.7 (9)
B3^ii—O1—O6^v	158.1 (2)	O2^viii—O8—O3^ii	107.7 (3)
B3^ii—O1—O9^iv	86.1 (4)	O2^viii—O8—O5^ii	164.5 (3)
O2—O1—O3	59.4 (4)	O2^viii—O8—O6	106.1 (4)
O2—O1—O4	139.0 (3)	O2^viii—O8—O7^ix	118.8 (3)
O2—O1—O5	119.0 (6)	O2^viii—O8—O7^vii	95.2 (3)
O2—O1—O6^v	102.4 (4)	O3^ii—O8—O5^ii	60.6 (3)
O2—O1—O9^iv	159.6 (2)	O3^ii—O8—O6	58.1 (3)
O3—O1—O4	98.3 (5)	O3^ii—O8—O7^ix	127.6 (6)
O3—O1—O5	59.9 (4)	O3^ii—O8—O7^vii	73.6 (4)
O3—O1—O6^v	149.6 (2)	O5^ii—O8—O6	59.6 (3)
O3—O1—O9^iv	116.5 (6)	O5^ii—O8—O7^ix	76.2 (3)
O4—O1—O5	56.7 (4)	O5^ii—O8—O7^vii	91.0 (5)
O4—O1—O6^v	79.8 (4)	O6—O8—O7^ix	123.1 (2)
O4—O1—O9^iv	59.27 (17)	O6—O8—O7^vii	131.0 (5)
O5—O1—O6^v	134.3 (3)	O7^ix—O8—O7^vii	79.4 (3)
O5—O1—O9^iv	58.8 (4)	Ca^ii—O9—B2^ix	95.3 (10)
O6^v—O1—O9^iv	88.8 (4)	Ca^ii—O9—O1^ix	123.1 (6)
B1—O2—O1	31.3 (8)	Ca^ii—O9—O2	95.7 (2)
B1—O2—O2^vi	89.3 (5)	Ca^ii—O9—O4^ix	94.2 (4)
B1—O2—O3	28.9 (8)	Ca^ii—O9—O4^v	112.5 (2)
B1—O2—O7^v	130.3 (9)	Ca^ii—O9—O5^ix	61.8 (4)
B1—O2—O8^iii	107.3 (9)	B2^ix—O9—O1^ix	35.0 (6)
B1—O2—O9	89.7 (5)	B2^ix—O9—O2	154.5 (3)
O1—O2—O2^vi	71.8 (2)	B2^ix—O9—O4^ix	35.2 (4)
O1—O2—O3	60.2 (4)	B2^ix—O9—O4^v	127.0 (8)
O1—O2—O7^v	99.8 (5)	B2^ix—O9—O5^ix	36.5 (9)
O1—O2—O8^iii	134.7 (5)	O1^ix—O9—O2	121.7 (3)
O1—O2—O9	105.6 (2)	O1^ix—O9—O4^ix	61.25 (18)
O2^vi—O2—O3	106.9 (3)	O1^ix—O9—O4^v	120.1 (5)
O2^vi—O2—O7^v	75.4 (4)	O1^ix—O9—O5^ix	61.7 (4)
O2^vi—O2—O8^iii	100.4 (2)	O2—O9—O4^ix	164.2 (6)
O2^vi—O2—O9	176.1 (4)	O2—O9—O4^v	68.6 (3)
O3—O2—O7^v	156.3 (3)	O2—O9—O5^ix	137.6 (4)
O3—O2—O8^iii	81.5 (4)	O4^ix—O9—O4^v	96.2 (4)
O3—O2—O9	73.7 (3)	O4^ix—O9—O5^ix	58.3 (4)
O7^v—O2—O8^iii	121.8 (3)	O4^v—O9—O5^ix	151.4 (2)

Symmetry codes: (i) −x, −y+1, −z; (ii) −x, −y+1, −z+1; (iii) x, y+1, z; (iv) x, y, z−1; (v) −x+1, −y+1, −z+1; (vi) −x+1, −y+2, −z+1; (vii) −x, −y, −z+1; (viii) x, y−1, z; (ix) x, y, z+1.

(II_3.75GPa)

Crystal data

H7B3CaO9	Z = 2
Mr = 223.6	F(000) = 214
Triclinic, P1	Dx = 2.468 Mg m^−3
Hall symbol: -P 1	Synchrotron radiation, λ = 0.41066 Å
a = 6.124 (3) Å	Cell parameters from 645 reflections
b = 7.6014 (3) Å	θ = 1.6–19.9°
c = 6.8051 (3) Å	µ = 0.25 mm^−1
α = 97.548 (4)°	T = 293 K
β = 107.416 (15)°	Prismatic habit, colourless
γ = 100.462 (12)°	0.02 × 0.01 × 0.01 mm
V = 291.36 (15) Å^3

Data collection

Beamline diffractometer	405 reflections with I > 3σ(I)
Radiation source: ESRF: Synchrotron radiation, undulator, IVU20c	Rint = 0.017
Silicon monochromator	θmax = 19.9°, θmin = 1.9°
ω scans	h = −3→4
645 measured reflections	k = −11→10
436 independent reflections	l = −10→10

Refinement

Refinement on F	0 constraints
R[F^2 > 2σ(F^2)] = 0.045	H-atom parameters not defined
wR(F^2) = 0.060	Weighting scheme based on measured s.u.'s w = 1/(σ^2(F) + 0.0001F^2)
S = 3.21	(Δ/σ)max = 0.025
436 reflections	Δρmax = 0.32 e Å^−3
53 parameters	Δρmin = −0.25 e Å^−3
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.4944 (5)	0.36149 (12)	0.71517 (16)	0.0102 (3)*
B1	0.303 (3)	0.8959 (7)	0.6398 (9)	0.0101 (10)*
B2	0.240 (4)	0.6381 (8)	0.8296 (11)	0.0105 (10)*
B3	0.648 (3)	0.7770 (7)	0.8371 (9)	0.0106 (10)*
O1	0.159 (2)	0.7776 (5)	0.7241 (6)	0.0117 (7)*
O2	0.270 (2)	0.8166 (4)	0.4184 (6)	0.0106 (7)*
O3	0.555 (2)	0.9322 (4)	0.7656 (6)	0.0108 (7)*
O4	0.1440 (19)	0.4551 (4)	0.6888 (6)	0.0128 (8)*
O5	0.490 (2)	0.6622 (4)	0.9121 (7)	0.0105 (7)*
O6	0.695 (2)	0.6618 (5)	0.6640 (6)	0.0117 (7)*
O7	0.2283 (19)	0.0717 (4)	0.6407 (6)	0.0104 (7)*
O8	0.879 (2)	0.8519 (4)	0.0106 (6)	0.0121 (7)*
O9	0.1523 (19)	0.6362 (4)	0.0134 (6)	0.0098 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
?	?	?	?	?	?	?

Geometric parameters (Å, º)

Ca1—B2	2.988 (19)	O1—O4	2.415 (6)
Ca1—O2^i	2.431 (11)	O1—O4^v	2.974 (6)
Ca1—O4	2.345 (12)	O1—O5	2.430 (15)
Ca1—O5	2.503 (6)	O1—O6^vi	2.701 (17)
Ca1—O5^ii	2.540 (6)	O1—O7^iii	2.373 (5)
Ca1—O6	2.508 (6)	O1—O9^iv	2.371 (7)
Ca1—O6^i	2.459 (4)	O2—O3	2.415 (8)
Ca1—O7	2.382 (6)	O2—O3^vii	2.653 (9)
Ca1—O9^i	2.383 (9)	O2—O4^v	2.797 (12)
B1—B2	2.519 (10)	O2—O7^iii	2.399 (9)
B1—B3	2.53 (2)	O2—O9	2.730 (5)
B1—O1	1.440 (16)	O3—O5	2.418 (6)
B1—O2	1.486 (9)	O3—O6	2.461 (11)
B1—O3	1.48 (2)	O3—O7^iii	2.418 (14)
B1—O5	2.868 (10)	O3—O8^iv	2.409 (12)
B1—O7^iii	1.489 (12)	O4—O4^v	2.893 (8)
B2—B3	2.51 (3)	O4—O5	2.346 (11)
B2—O1	1.439 (12)	O4—O6^i	2.948 (12)
B2—O3	2.847 (17)	O4—O9^iv	2.426 (8)
B2—O4	1.488 (6)	O5—O5^ii	2.886 (6)
B2—O5	1.43 (3)	O5—O6	2.390 (15)
B2—O9^iv	1.504 (18)	O5—O8^iv	2.398 (15)
B3—O1	2.86 (2)	O5—O9^iv	2.349 (18)
B3—O3	1.476 (12)	O6—O8^iv	2.417 (5)
B3—O5	1.439 (17)	O7—O7^viii	2.795 (13)
B3—O6	1.505 (14)	O7—O8^i	2.665 (11)
B3—O8^iv	1.499 (15)	O8—O8^ix	2.509 (9)
O1—O2	2.412 (11)	O8—O9^x	2.546 (13)
O1—O3	2.415 (16)	O9—O9^xi	2.469 (10)
B2—Ca1—O2^i	167.8 (3)	O1—O3—O7^iii	58.8 (4)
B2—Ca1—O4	29.4 (3)	O1—O3—O8^iv	118.7 (3)
B2—Ca1—O5	28.4 (4)	O2—O3—O2^vii	83.4 (2)
B2—Ca1—O5^ii	76.0 (3)	O2—O3—O5	98.4 (3)
B2—Ca1—O6	72.9 (4)	O2—O3—O6	80.8 (3)
B2—Ca1—O6^i	93.0 (3)	O2—O3—O7^iii	59.5 (3)
B2—Ca1—O7	106.2 (4)	O2—O3—O8^iv	140.1 (4)
B2—Ca1—O9^i	113.7 (3)	O2^vii—O3—O5	162.5 (7)
O2^i—Ca1—O4	152.60 (19)	O2^vii—O3—O6	104.8 (5)
O2^i—Ca1—O5	145.9 (4)	O2^vii—O3—O7^iii	77.9 (3)
O2^i—Ca1—O5^ii	113.7 (3)	O2^vii—O3—O8^iv	108.4 (5)
O2^i—Ca1—O6	95.6 (3)	O5—O3—O6	58.7 (3)
O2^i—Ca1—O6^i	80.5 (3)	O5—O3—O7^iii	118.1 (6)
O2^i—Ca1—O7	83.1 (3)	O5—O3—O8^iv	59.6 (4)
O2^i—Ca1—O9^i	69.1 (2)	O6—O3—O7^iii	139.9 (3)
O4—Ca1—O5	57.8 (3)	O6—O3—O8^iv	59.5 (3)
O4—Ca1—O5^ii	85.0 (3)	O7^iii—O3—O8^iv	158.8 (4)
O4—Ca1—O6	92.9 (3)	Ca1—O4—B2	100.0 (10)
O4—Ca1—O6^i	75.7 (3)	Ca1—O4—O1	117.9 (5)
O4—Ca1—O7	80.2 (3)	Ca1—O4—O1^v	99.0 (3)
O4—Ca1—O9^i	137.2 (2)	Ca1—O4—O2^v	117.6 (2)
O5—Ca1—O5^ii	69.80 (17)	Ca1—O4—O4^v	123.4 (4)
O5—Ca1—O6	57.0 (3)	Ca1—O4—O5	64.5 (4)
O5—Ca1—O6^i	109.9 (2)	Ca1—O4—O6^i	53.9 (3)
O5—Ca1—O7	129.7 (4)	Ca1—O4—O9^iv	113.3 (4)
O5—Ca1—O9^i	88.6 (3)	B2—O4—O1	33.8 (5)
O5^ii—Ca1—O6	116.75 (15)	B2—O4—O1^v	149.8 (6)
O5^ii—Ca1—O6^i	156.0 (4)	B2—O4—O2^v	135.3 (11)
O5^ii—Ca1—O7	81.33 (19)	B2—O4—O4^v	101.2 (5)
O5^ii—Ca1—O9^i	56.9 (4)	B2—O4—O5	35.5 (10)
O6—Ca1—O6^i	78.96 (17)	B2—O4—O6^i	123.4 (9)
O6—Ca1—O7	160.21 (16)	B2—O4—O9^iv	36.0 (7)
O6—Ca1—O9^i	88.6 (2)	O1—O4—O1^v	116.1 (3)
O6^i—Ca1—O7	81.36 (18)	O1—O4—O2^v	124.2 (6)
O6^i—Ca1—O9^i	145.8 (4)	O1—O4—O4^v	67.5 (2)
O7—Ca1—O9^i	109.2 (2)	O1—O4—O5	61.4 (3)
B2—B1—B3	59.6 (6)	O1—O4—O6^i	108.8 (3)
B2—B1—O1	28.9 (7)	O1—O4—O9^iv	58.6 (2)
B2—B1—O2	108.4 (3)	O1^v—O4—O2^v	49.3 (2)
B2—B1—O3	86.7 (6)	O1^v—O4—O4^v	48.59 (15)
B2—B1—O5	29.8 (6)	O1^v—O4—O5	152.9 (5)
B2—B1—O7^iii	132.8 (11)	O1^v—O4—O6^i	54.3 (3)
B3—B1—O1	87.9 (6)	O1^v—O4—O9^iv	145.8 (6)
B3—B1—O2	101.5 (9)	O2^v—O4—O4^v	78.4 (3)
B3—B1—O3	31.1 (3)	O2^v—O4—O5	156.8 (3)
B3—B1—O5	30.1 (4)	O2^v—O4—O6^i	99.0 (2)
B3—B1—O7^iii	138.3 (6)	O2^v—O4—O9^iv	102.9 (4)
O1—B1—O2	111.1 (6)	O4^v—O4—O5	121.0 (2)
O1—B1—O3	111.7 (6)	O4^v—O4—O6^i	70.7 (3)
O1—B1—O5	57.8 (6)	O4^v—O4—O9^iv	114.6 (4)
O1—B1—O7^iii	108.2 (13)	O5—O4—O6^i	99.6 (5)
O2—B1—O3	109.1 (13)	O5—O4—O9^iv	58.9 (4)
O2—B1—O5	110.2 (6)	O6^i—O4—O9^iv	158.1 (5)
O2—B1—O7^iii	107.5 (5)	Ca1—O5—Ca1^ii	110.20 (16)
O3—B1—O5	57.4 (4)	Ca1—O5—B1	112.8 (2)
O3—B1—O7^iii	109.2 (6)	Ca1—O5—B2	95.0 (4)
O5—B1—O7^iii	142.3 (4)	Ca1—O5—B3	97.8 (6)
Ca1—B2—B1	108.5 (8)	Ca1—O5—O1	111.5 (2)
Ca1—B2—B3	66.8 (6)	Ca1—O5—O3	119.2 (4)
Ca1—B2—O1	130.9 (9)	Ca1—O5—O4	57.7 (3)
Ca1—B2—O3	93.3 (7)	Ca1—O5—O5^ii	55.70 (16)
Ca1—B2—O4	50.6 (8)	Ca1—O5—O6	61.6 (2)
Ca1—B2—O5	56.6 (6)	Ca1—O5—O8^iv	106.8 (5)
Ca1—B2—O9^iv	121.5 (5)	Ca1—O5—O9^iv	110.4 (3)
B1—B2—B3	60.4 (6)	Ca1^ii—O5—B1	132.5 (5)
B1—B2—O1	28.9 (8)	Ca1^ii—O5—B2	95.8 (7)
B1—B2—O3	31.2 (4)	Ca1^ii—O5—B3	130.3 (5)
B1—B2—O4	113.8 (5)	Ca1^ii—O5—O1	113.2 (5)
B1—B2—O5	88.8 (8)	Ca1^ii—O5—O3	129.0 (2)
B1—B2—O9^iv	128.1 (8)	Ca1^ii—O5—O4	106.4 (4)
B3—B2—O1	88.7 (9)	Ca1^ii—O5—O5^ii	54.51 (16)
B3—B2—O3	31.2 (4)	Ca1^ii—O5—O6	146.5 (6)
B3—B2—O4	111.7 (12)	Ca1^ii—O5—O8^iv	95.3 (3)
B3—B2—O5	29.0 (5)	Ca1^ii—O5—O9^iv	58.2 (3)
B3—B2—O9^iv	127.3 (7)	B1—O5—B2	61.4 (5)
O1—B2—O3	58.0 (7)	B1—O5—B3	61.7 (7)
O1—B2—O4	111.2 (7)	B1—O5—O1	30.1 (4)
O1—B2—O5	116.0 (11)	B1—O5—O3	31.0 (4)
O1—B2—O9^iv	107.3 (13)	B1—O5—O4	80.9 (3)
O3—B2—O4	124.9 (10)	B1—O5—O5^ii	158.4 (5)
O3—B2—O5	58.1 (6)	B1—O5—O6	74.8 (4)
O3—B2—O9^iv	126.6 (4)	B1—O5—O8^iv	91.0 (4)
O4—B2—O5	107.2 (13)	B1—O5—O9^iv	88.0 (5)
O4—B2—O9^iv	108.4 (10)	B2—O5—B3	122.3 (8)
O5—B2—O9^iv	106.6 (7)	B2—O5—O1	32.2 (4)
B1—B3—B2	60.0 (6)	B2—O5—O3	91.8 (5)
B1—B3—O1	30.2 (4)	B2—O5—O4	37.3 (4)
B1—B3—O3	31.2 (6)	B2—O5—O5^ii	99.5 (5)
B1—B3—O5	88.2 (10)	B2—O5—O6	116.7 (6)
B1—B3—O6	102.9 (5)	B2—O5—O8^iv	150.2 (4)
B1—B3—O8^iv	137.5 (5)	B2—O5—O9^iv	37.9 (6)
B2—B3—O1	30.2 (3)	B3—O5—O1	91.9 (7)
B2—B3—O3	87.1 (10)	B3—O5—O3	34.4 (7)
B2—B3—O5	28.7 (6)	B3—O5—O4	123.3 (4)
B2—B3—O6	107.3 (6)	B3—O5—O5^ii	133.4 (10)
B2—B3—O8^iv	133.4 (7)	B3—O5—O6	36.6 (4)
O1—B3—O3	57.5 (8)	B3—O5—O8^iv	36.1 (5)
O1—B3—O5	58.0 (8)	B3—O5—O9^iv	145.2 (8)
O1—B3—O6	110.7 (7)	O1—O5—O3	59.8 (4)
O1—B3—O8^iv	142.2 (8)	O1—O5—O4	60.7 (3)
O3—B3—O5	112.1 (14)	O1—O5—O5^ii	131.6 (5)
O3—B3—O6	111.3 (5)	O1—O5—O6	99.4 (3)
O3—B3—O8^iv	108.1 (5)	O1—O5—O8^iv	118.6 (3)
O5—B3—O6	108.6 (5)	O1—O5—O9^iv	59.5 (4)
O5—B3—O8^iv	109.4 (5)	O3—O5—O4	109.7 (3)
O6—B3—O8^iv	107.2 (13)	O3—O5—O5^ii	167.8 (7)
B1—O1—B2	122.1 (14)	O3—O5—O6	61.6 (3)
B1—O1—B3	61.9 (8)	O3—O5—O8^iv	60.0 (3)
B1—O1—O2	35.1 (3)	O3—O5—O9^iv	111.2 (5)
B1—O1—O3	34.7 (6)	O4—O5—O5^ii	77.6 (2)
B1—O1—O4	122.0 (8)	O4—O5—O6	96.0 (3)
B1—O1—O4^v	95.5 (3)	O4—O5—O8^iv	156.6 (5)
B1—O1—O5	92.1 (9)	O4—O5—O9^iv	62.2 (4)
B1—O1—O6^vi	137.4 (7)	O5^ii—O5—O6	108.8 (4)
B1—O1—O7^iii	36.6 (6)	O5^ii—O5—O8^iv	109.4 (5)
B1—O1—O9^iv	144.9 (8)	O5^ii—O5—O9^iv	80.7 (4)
B2—O1—B3	61.2 (10)	O6—O5—O8^iv	60.6 (4)
B2—O1—O2	115.9 (10)	O6—O5—O9^iv	154.5 (4)
B2—O1—O3	91.7 (10)	O8^iv—O5—O9^iv	139.9 (3)
B2—O1—O4	35.1 (3)	Ca1—O6—Ca1^i	101.0 (2)
B2—O1—O4^v	99.0 (3)	Ca1—O6—B3	95.8 (5)
B2—O1—O5	31.8 (9)	Ca1—O6—O1^x	126.7 (4)
B2—O1—O6^vi	98.2 (10)	Ca1—O6—O3	117.4 (5)
B2—O1—O7^iii	150.9 (10)	Ca1—O6—O4^i	101.51 (18)
B2—O1—O9^iv	37.3 (8)	Ca1—O6—O5	61.4 (2)
B3—O1—O2	73.5 (4)	Ca1—O6—O8^iv	106.1 (2)
B3—O1—O3	31.0 (2)	Ca1^i—O6—B3	125.9 (7)
B3—O1—O4	78.5 (4)	Ca1^i—O6—O1^x	103.8 (3)
B3—O1—O4^v	115.2 (4)	Ca1^i—O6—O3	94.3 (3)
B3—O1—O5	30.1 (3)	Ca1^i—O6—O4^i	50.4 (2)
B3—O1—O6^vi	159.1 (2)	Ca1^i—O6—O5	123.9 (5)
B3—O1—O7^iii	91.7 (5)	Ca1^i—O6—O8^iv	148.6 (2)
B3—O1—O9^iv	87.1 (4)	B3—O6—O1^x	106.0 (7)
O2—O1—O3	60.0 (3)	B3—O6—O3	34.0 (3)
O2—O1—O4	96.4 (3)	B3—O6—O4^i	162.7 (5)
O2—O1—O4^v	61.5 (3)	B3—O6—O5	34.8 (5)
O2—O1—O5	98.1 (6)	B3—O6—O8^iv	36.3 (7)
O2—O1—O6^vi	117.3 (3)	O1^x—O6—O3	106.9 (3)
O2—O1—O7^iii	60.2 (3)	O1^x—O6—O4^i	63.4 (3)
O2—O1—O9^iv	153.1 (5)	O1^x—O6—O5	130.1 (3)
O3—O1—O4	107.5 (6)	O1^x—O6—O8^iv	72.1 (4)
O3—O1—O4^v	119.2 (4)	O3—O6—O4^i	132.7 (2)
O3—O1—O5	59.9 (4)	O3—O6—O5	59.8 (3)
O3—O1—O6^vi	169.7 (3)	O3—O6—O8^iv	59.2 (3)
O3—O1—O7^iii	60.7 (4)	O4^i—O6—O5	162.1 (3)
O3—O1—O9^iv	110.6 (4)	O4^i—O6—O8^iv	135.4 (6)
O4—O1—O4^v	63.94 (18)	O5—O6—O8^iv	59.8 (3)
O4—O1—O5	57.9 (3)	Ca1—O7—B1^xii	123.6 (9)
O4—O1—O6^vi	82.4 (4)	Ca1—O7—O1^xii	146.7 (4)
O4—O1—O7^iii	156.4 (5)	Ca1—O7—O2^xii	120.3 (5)
O4—O1—O9^iv	60.9 (2)	Ca1—O7—O3^xii	90.2 (4)
O4^v—O1—O5	115.0 (3)	Ca1—O7—O7^viii	132.5 (2)
O4^v—O1—O6^vi	62.4 (3)	Ca1—O7—O8^i	92.52 (18)
O4^v—O1—O7^iii	102.47 (19)	B1^xii—O7—O1^xii	35.2 (7)
O4^v—O1—O9^iv	113.5 (3)	B1^xii—O7—O2^xii	36.2 (3)
O5—O1—O6^vi	129.7 (3)	B1^xii—O7—O3^xii	35.3 (6)
O5—O1—O7^iii	119.5 (5)	B1^xii—O7—O7^viii	96.7 (6)
O5—O1—O9^iv	58.6 (4)	B1^xii—O7—O8^i	107.8 (5)
O6^vi—O1—O7^iii	109.1 (5)	O1^xii—O7—O2^xii	60.7 (3)
O6^vi—O1—O9^iv	76.2 (4)	O1^xii—O7—O3^xii	60.5 (4)
O7^iii—O1—O9^iv	140.7 (2)	O1^xii—O7—O7^viii	80.7 (3)
Ca1^i—O2—B1	128.6 (8)	O1^xii—O7—O8^i	79.3 (3)
Ca1^i—O2—O1	124.4 (3)	O2^xii—O7—O3^xii	60.2 (3)
Ca1^i—O2—O3	96.2 (5)	O2^xii—O7—O7^viii	76.8 (3)
Ca1^i—O2—O3^vii	83.8 (4)	O2^xii—O7—O8^i	140.0 (2)
Ca1^i—O2—O4^v	98.7 (2)	O3^xii—O7—O7^viii	131.8 (2)
Ca1^i—O2—O7^iii	152.3 (5)	O3^xii—O7—O8^i	101.1 (3)
Ca1^i—O2—O9	54.6 (3)	O7^viii—O7—O8^i	98.4 (5)
B1—O2—O1	33.8 (5)	B3^xiii—O8—O3^xiii	35.6 (3)
B1—O2—O3	35.3 (8)	B3^xiii—O8—O5^xiii	34.5 (5)
B1—O2—O3^vii	110.6 (4)	B3^xiii—O8—O6^xiii	36.5 (7)
B1—O2—O4^v	101.8 (8)	B3^xiii—O8—O7^i	105.8 (8)
B1—O2—O7^iii	36.3 (4)	B3^xiii—O8—O8^ix	116.5 (4)
B1—O2—O9	171.6 (8)	B3^xiii—O8—O9^x	110.8 (5)
O1—O2—O3	60.0 (4)	O3^xiii—O8—O5^xiii	60.4 (3)
O1—O2—O3^vii	142.8 (2)	O3^xiii—O8—O6^xiii	61.3 (3)
O1—O2—O4^v	69.2 (3)	O3^xiii—O8—O7^i	99.0 (5)
O1—O2—O7^iii	59.1 (2)	O3^xiii—O8—O8^ix	85.4 (3)
O1—O2—O9	137.9 (4)	O3^xiii—O8—O9^x	139.1 (2)
O3—O2—O3^vii	96.6 (3)	O5^xiii—O8—O6^xiii	59.5 (3)
O3—O2—O4^v	126.4 (3)	O5^xiii—O8—O7^i	78.5 (4)
O3—O2—O7^iii	60.3 (3)	O5^xiii—O8—O8^ix	145.5 (4)
O3—O2—O9	150.4 (6)	O5^xiii—O8—O9^x	106.2 (3)
O3^vii—O2—O4^v	135.9 (3)	O6^xiii—O8—O7^i	138.0 (5)
O3^vii—O2—O7^iii	84.5 (2)	O6^xiii—O8—O8^ix	109.9 (3)
O3^vii—O2—O9	76.8 (2)	O6^xiii—O8—O9^x	78.4 (3)
O4^v—O2—O7^iii	107.1 (5)	O7^i—O8—O8^ix	104.5 (2)
O4^v—O2—O9	69.8 (3)	O7^i—O8—O9^x	116.8 (3)
O7^iii—O2—O9	145.0 (4)	O8^ix—O8—O9^x	102.8 (5)
B1—O3—B2	62.1 (5)	Ca1^i—O9—B2^xiii	100.3 (9)
B1—O3—B3	117.7 (7)	Ca1^i—O9—O1^xiii	121.6 (5)
B1—O3—O1	33.6 (4)	Ca1^i—O9—O2	56.3 (3)
B1—O3—O2	35.5 (5)	Ca1^i—O9—O4^xiii	108.9 (5)
B1—O3—O2^vii	99.6 (4)	Ca1^i—O9—O5^xiii	64.9 (3)
B1—O3—O5	91.6 (5)	Ca1^i—O9—O8^vi	127.93 (18)
B1—O3—O6	106.8 (4)	Ca1^i—O9—O9^xi	109.2 (2)
B1—O3—O7^iii	35.6 (3)	B2^xiii—O9—O1^xiii	35.4 (6)
B1—O3—O8^iv	151.1 (4)	B2^xiii—O9—O2	139.7 (7)
B2—O3—B3	61.7 (8)	B2^xiii—O9—O4^xiii	35.6 (3)
B2—O3—O1	30.3 (4)	B2^xiii—O9—O5^xiii	35.6 (8)
B2—O3—O2	77.3 (3)	B2^xiii—O9—O8^vi	110.9 (6)
B2—O3—O2^vii	160.3 (4)	B2^xiii—O9—O9^xi	115.7 (4)
B2—O3—O5	30.1 (5)	O1^xiii—O9—O2	125.04 (17)
B2—O3—O6	76.2 (4)	O1^xiii—O9—O4^xiii	60.4 (2)
B2—O3—O7^iii	88.8 (6)	O1^xiii—O9—O5^xiii	62.0 (4)
B2—O3—O8^iv	89.2 (4)	O1^xiii—O9—O8^vi	75.7 (3)
B3—O3—O1	91.5 (8)	O1^xiii—O9—O9^xi	122.8 (3)
B3—O3—O2	107.0 (3)	O2—O9—O4^xiii	165.2 (6)
B3—O3—O2^vii	129.4 (10)	O2—O9—O5^xiii	109.9 (4)
B3—O3—O5	33.4 (8)	O2—O9—O8^vi	73.4 (3)
B3—O3—O6	34.7 (4)	O2—O9—O9^xi	103.7 (3)
B3—O3—O7^iii	150.3 (9)	O4^xiii—O9—O5^xiii	58.8 (3)
B3—O3—O8^iv	36.3 (5)	O4^xiii—O9—O8^vi	120.9 (3)
O1—O3—O2	59.9 (3)	O4^xiii—O9—O9^xi	80.5 (3)
O1—O3—O2^vii	132.9 (4)	O5^xiii—O9—O8^vi	130.2 (3)
O1—O3—O5	60.4 (4)	O5^xiii—O9—O9^xi	130.3 (3)
O1—O3—O6	97.8 (3)	O8^vi—O9—O9^xi	93.7 (5)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y+1, −z+2; (iii) x, y+1, z; (iv) x, y, z+1; (v) −x, −y+1, −z+1; (vi) x−1, y, z; (vii) −x+1, −y+2, −z+1; (viii) −x, −y, −z+1; (ix) −x+2, −y+2, −z; (x) x+1, y, z; (xi) −x, −y+1, −z; (xii) x, y−1, z; (xiii) x, y, z−1.

(II_5.10GPa)

Crystal data

H7B3CaO9	Z = 2
Mr = 223.6	F(000) = 214
Triclinic, P1	Dx = 2.508 Mg m^−3
Hall symbol: -P 1	Synchrotron radiation, λ = 0.41066 Å
a = 6.095 (3) Å	Cell parameters from 612 reflections
b = 7.5590 (2) Å	θ = 2.7–19.9°
c = 6.7696 (2) Å	µ = 0.25 mm^−1
α = 97.576 (3)°	T = 293 K
β = 107.579 (14)°	Prismatic habit, colourless
γ = 100.340 (11)°	0.02 × 0.01 × 0.01 mm
V = 286.68 (14) Å^3

Data collection

Beamline diffractometer	386 reflections with I > 3σ(I)
Radiation source: ESRF: Synchrotron radiation, undulator, IVU20c	Rint = 0.013
Silicon monochromator	θmax = 19.9°, θmin = 2.7°
ω scans	h = −3→3
612 measured reflections	k = −12→12
414 independent reflections	l = −11→10

Refinement

Refinement on F	0 constraints
R[F^2 > 2σ(F^2)] = 0.051	H-atom parameters not defined
wR(F^2) = 0.065	Weighting scheme based on measured s.u.'s w = 1/(σ^2(F) + 0.0001F^2)
S = 3.49	(Δ/σ)max = 0.036
414 reflections	Δρmax = 0.32 e Å^−3
53 parameters	Δρmin = −0.33 e Å^−3
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.4921 (6)	0.36229 (14)	0.71429 (19)	0.0115 (3)*
B1	0.299 (3)	0.8952 (7)	0.6411 (10)	0.0085 (10)*
B2	0.231 (5)	0.6373 (9)	0.8289 (13)	0.0122 (12)*
B3	0.651 (4)	0.7783 (8)	0.8397 (11)	0.0127 (12)*
O1	0.155 (2)	0.7784 (5)	0.7238 (7)	0.0129 (9)*
O2	0.270 (2)	0.8162 (5)	0.4179 (7)	0.0117 (8)*
O3	0.558 (2)	0.9342 (5)	0.7679 (7)	0.0121 (8)*
O4	0.136 (2)	0.4545 (5)	0.6862 (7)	0.0133 (9)*
O5	0.493 (3)	0.6641 (6)	0.9131 (8)	0.0128 (9)*
O6	0.696 (2)	0.6616 (5)	0.6643 (7)	0.0120 (8)*
O7	0.232 (2)	0.0744 (5)	0.6397 (7)	0.0105 (8)*
O8	0.879 (2)	0.8523 (5)	0.0129 (7)	0.0122 (8)*
O9	0.147 (2)	0.6357 (5)	0.0141 (7)	0.0109 (8)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
?	?	?	?	?	?	?

Geometric parameters (Å, º)

Ca1—O2^i	2.427 (13)	O1—O2	2.414 (13)
Ca1—O4	2.359 (15)	O1—O3	2.438 (19)
Ca1—O5	2.489 (7)	O1—O4	2.407 (7)
Ca1—O6	2.495 (7)	O1—O5	2.447 (17)
Ca1—O6^i	2.438 (5)	O1—O7^ii	2.381 (6)
Ca1—O7	2.343 (7)	O1—O9^iii	2.372 (8)
Ca1—O9^i	2.398 (10)	O2—O3	2.420 (9)
B1—O1	1.419 (18)	O2—O7^ii	2.390 (10)
B1—O2	1.495 (10)	O3—O5	2.401 (7)
B1—O3	1.51 (2)	O3—O6	2.458 (13)
B1—O7^ii	1.481 (13)	O3—O7^ii	2.402 (16)
B2—O1	1.429 (13)	O3—O8^iii	2.390 (14)
B2—O4	1.483 (8)	O4—O5	2.391 (14)
B2—O5	1.49 (3)	O4—O9^iii	2.425 (9)
B2—O9^iii	1.49 (2)	O5—O6	2.370 (18)
B3—O3	1.474 (14)	O5—O8^iii	2.365 (18)
B3—O5	1.42 (2)	O5—O9^iii	2.39 (2)
B3—O6	1.507 (17)	O6—O8^iii	2.414 (6)
B3—O8^iii	1.478 (18)	O9—O9^iv	2.416 (12)
O2^i—Ca1—O4	152.5 (2)	O5—O3—O6	58.4 (4)
O2^i—Ca1—O5	144.9 (4)	O5—O3—O7^ii	118.7 (7)
O2^i—Ca1—O6	95.2 (4)	O5—O3—O8^iii	59.2 (4)
O2^i—Ca1—O6^i	80.4 (3)	O6—O3—O7^ii	139.3 (3)
O2^i—Ca1—O7	82.7 (4)	O6—O3—O8^iii	59.7 (3)
O2^i—Ca1—O9^i	68.1 (3)	O7^ii—O3—O8^iii	159.3 (4)
O4—Ca1—O5	59.0 (4)	Ca1—O4—B2	99.8 (12)
O4—Ca1—O6	93.8 (4)	Ca1—O4—O1	116.8 (6)
O4—Ca1—O6^i	75.9 (4)	Ca1—O4—O5	63.2 (5)
O4—Ca1—O7	80.2 (3)	Ca1—O4—O9^iii	112.6 (4)
O4—Ca1—O9^i	138.2 (3)	B2—O4—O1	33.6 (5)
O5—Ca1—O6	56.8 (4)	B2—O4—O5	36.6 (12)
O5—Ca1—O6^i	110.5 (2)	B2—O4—O9^iii	35.5 (8)
O5—Ca1—O7	131.0 (5)	O1—O4—O5	61.3 (4)
O5—Ca1—O9^i	88.3 (3)	O1—O4—O9^iii	58.8 (2)
O6—Ca1—O6^i	79.2 (2)	O5—O4—O9^iii	59.5 (4)
O6—Ca1—O7	160.53 (18)	Ca1—O5—B2	94.2 (5)
O6—Ca1—O9^i	87.8 (3)	Ca1—O5—B3	98.5 (8)
O6^i—Ca1—O7	81.4 (2)	Ca1—O5—O1	110.7 (3)
O6^i—Ca1—O9^i	144.7 (5)	Ca1—O5—O3	119.6 (4)
O7—Ca1—O9^i	109.1 (2)	Ca1—O5—O4	57.8 (3)
O1—B1—O2	111.9 (6)	Ca1—O5—O6	61.7 (3)
O1—B1—O3	112.9 (7)	Ca1—O5—O8^iii	107.8 (7)
O1—B1—O7^ii	110.4 (14)	Ca1—O5—O9^iii	109.3 (4)
O2—B1—O3	107.5 (14)	B2—O5—B3	123.4 (9)
O2—B1—O7^ii	106.8 (6)	B2—O5—O1	32.3 (4)
O3—B1—O7^ii	107.0 (7)	B2—O5—O3	92.6 (6)
O1—B2—O4	111.4 (8)	B2—O5—O4	36.4 (5)
O1—B2—O5	113.9 (13)	B2—O5—O6	117.2 (6)
O1—B2—O9^iii	108.6 (16)	B2—O5—O8^iii	150.9 (5)
O4—B2—O5	107.0 (15)	B2—O5—O9^iii	36.8 (6)
O4—B2—O9^iii	109.2 (11)	B3—O5—O1	92.7 (8)
O5—B2—O9^iii	106.5 (9)	B3—O5—O3	34.7 (8)
O3—B3—O5	112.1 (17)	B3—O5—O4	124.0 (5)
O3—B3—O6	111.1 (6)	B3—O5—O6	37.2 (5)
O3—B3—O8^iii	108.1 (6)	B3—O5—O8^iii	36.1 (6)
O5—B3—O6	108.1 (6)	B3—O5—O9^iii	145.4 (9)
O5—B3—O8^iii	109.4 (7)	O1—O5—O3	60.4 (4)
O6—B3—O8^iii	108.0 (16)	O1—O5—O4	59.7 (4)
B1—O1—B2	123.1 (17)	O1—O5—O6	99.8 (4)
B1—O1—O2	35.1 (3)	O1—O5—O8^iii	119.3 (3)
B1—O1—O3	34.7 (7)	O1—O5—O9^iii	58.7 (5)
B1—O1—O4	122.2 (9)	O3—O5—O4	109.6 (4)
B1—O1—O5	91.0 (10)	O3—O5—O6	62.0 (4)
B1—O1—O7^ii	35.7 (7)	O3—O5—O8^iii	60.2 (4)
B1—O1—O9^iii	144.9 (9)	O3—O5—O9^iii	111.2 (6)
B2—O1—O2	116.0 (12)	O4—O5—O6	96.3 (4)
B2—O1—O3	92.6 (12)	O4—O5—O8^iii	157.5 (6)
B2—O1—O4	35.0 (4)	O4—O5—O9^iii	61.0 (5)
B2—O1—O5	33.8 (11)	O6—O5—O8^iii	61.3 (5)
B2—O1—O7^ii	151.1 (12)	O6—O5—O9^iii	153.9 (5)
B2—O1—O9^iii	36.6 (10)	O8^iii—O5—O9^iii	140.1 (4)
O2—O1—O3	59.8 (4)	Ca1—O6—Ca1^i	100.8 (2)
O2—O1—O4	96.1 (4)	Ca1—O6—B3	95.8 (7)
O2—O1—O5	96.9 (7)	Ca1—O6—O3	117.1 (6)
O2—O1—O7^ii	59.8 (3)	Ca1—O6—O5	61.5 (3)
O2—O1—O9^iii	152.6 (6)	Ca1—O6—O8^iii	106.0 (3)
O3—O1—O4	107.9 (7)	Ca1^i—O6—B3	126.6 (8)
O3—O1—O5	58.9 (4)	Ca1^i—O6—O3	94.8 (3)
O3—O1—O7^ii	59.8 (4)	Ca1^i—O6—O5	124.5 (7)
O3—O1—O9^iii	110.5 (5)	Ca1^i—O6—O8^iii	148.7 (2)
O4—O1—O5	59.0 (4)	B3—O6—O3	34.0 (4)
O4—O1—O7^ii	155.7 (6)	B3—O6—O5	34.7 (6)
O4—O1—O9^iii	61.0 (2)	B3—O6—O8^iii	35.6 (8)
O5—O1—O7^ii	117.7 (6)	O3—O6—O5	59.6 (4)
O5—O1—O9^iii	59.4 (5)	O3—O6—O8^iii	58.7 (3)
O7^ii—O1—O9^iii	141.1 (3)	O5—O6—O8^iii	59.2 (4)
Ca1^i—O2—B1	129.2 (9)	Ca1—O7—B1^v	126.3 (10)
Ca1^i—O2—O1	124.8 (3)	Ca1—O7—O1^v	147.9 (5)
Ca1^i—O2—O3	96.1 (5)	Ca1—O7—O2^v	121.6 (6)
Ca1^i—O2—O7^ii	151.4 (6)	Ca1—O7—O3^v	91.0 (5)
B1—O2—O1	33.0 (6)	B1^v—O7—O1^v	33.9 (8)
B1—O2—O3	36.4 (9)	B1^v—O7—O2^v	36.8 (3)
B1—O2—O7^ii	36.4 (4)	B1^v—O7—O3^v	36.8 (7)
O1—O2—O3	60.6 (4)	O1^v—O7—O2^v	60.8 (3)
O1—O2—O7^ii	59.4 (3)	O1^v—O7—O3^v	61.3 (4)
O3—O2—O7^ii	59.9 (4)	O2^v—O7—O3^v	60.7 (4)
B1—O3—B3	117.0 (8)	B3^vi—O8—O3^vi	35.9 (4)
B1—O3—O1	32.4 (5)	B3^vi—O8—O5^vi	34.5 (6)
B1—O3—O2	36.1 (6)	B3^vi—O8—O6^vi	36.4 (8)
B1—O3—O5	90.7 (6)	O3^vi—O8—O5^vi	60.7 (4)
B1—O3—O6	106.3 (5)	O3^vi—O8—O6^vi	61.6 (3)
B1—O3—O7^ii	36.1 (4)	O5^vi—O8—O6^vi	59.4 (4)
B1—O3—O8^iii	149.9 (5)	Ca1^i—O9—B2^vi	100.3 (11)
B3—O3—O1	91.8 (9)	Ca1^i—O9—O1^vi	120.7 (6)
B3—O3—O2	106.7 (4)	Ca1^i—O9—O4^vi	108.7 (6)
B3—O3—O5	33.2 (10)	Ca1^i—O9—O5^vi	63.9 (4)
B3—O3—O6	34.9 (5)	Ca1^i—O9—O9^iv	109.1 (3)
B3—O3—O7^ii	150.7 (11)	B2^vi—O9—O1^vi	34.8 (7)
B3—O3—O8^iii	36.0 (6)	B2^vi—O9—O4^vi	35.3 (4)
O1—O3—O2	59.6 (4)	B2^vi—O9—O5^vi	36.7 (10)
O1—O3—O5	60.8 (5)	B2^vi—O9—O9^iv	114.6 (5)
O1—O3—O6	97.6 (4)	O1^vi—O9—O4^vi	60.2 (2)
O1—O3—O7^ii	58.9 (4)	O1^vi—O9—O5^vi	61.8 (5)
O1—O3—O8^iii	118.7 (4)	O1^vi—O9—O9^iv	123.0 (4)
O2—O3—O5	98.0 (3)	O4^vi—O9—O5^vi	59.5 (4)
O2—O3—O6	80.2 (3)	O4^vi—O9—O9^iv	79.7 (3)
O2—O3—O7^ii	59.4 (4)	O5^vi—O9—O9^iv	129.6 (4)
O2—O3—O8^iii	139.7 (4)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, y+1, z; (iii) x, y, z+1; (iv) −x, −y+1, −z; (v) x, y−1, z; (vi) x, y, z−1.

(II_6.37GPa)

Crystal data

H7B3CaO9	Z = 2
Mr = 223.6	F(000) = 214
Triclinic, P1	Dx = 2.543 Mg m^−3
Hall symbol: -P 1	Synchrotron radiation, λ = 0.41066 Å
a = 6.071 (3) Å	Cell parameters from 595 reflections
b = 7.5224 (2) Å	θ = 2.7–20.0°
c = 6.7393 (2) Å	µ = 0.26 mm^−1
α = 97.606 (3)°	T = 293 K
β = 107.703 (14)°	Prismatic habit, colourless
γ = 100.254 (12)°	0.02 × 0.01 × 0.01 mm
V = 282.75 (14) Å^3

Data collection

Beamline diffractometer	375 reflections with I > 3σ(I)
Radiation source: ESRF: Synchrotron radiation, undulator, IVU20c	Rint = 0.015
Silicon monochromator	θmax = 20.0°, θmin = 2.7°
ω scans	h = −3→3
595 measured reflections	k = −12→12
400 independent reflections	l = −11→10

Refinement

Refinement on F	0 constraints
R[F^2 > 2σ(F^2)] = 0.039	H-atom parameters not defined
wR(F^2) = 0.052	Weighting scheme based on measured s.u.'s w = 1/(σ^2(F) + 0.0001F^2)
S = 2.92	(Δ/σ)max = 0.038
400 reflections	Δρmax = 0.22 e Å^−3
53 parameters	Δρmin = −0.21 e Å^−3
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.4936 (5)	0.36329 (11)	0.71396 (15)	0.0104 (3)*
B1	0.302 (3)	0.8980 (6)	0.6406 (8)	0.0084 (8)*
B2	0.235 (4)	0.6388 (7)	0.8300 (10)	0.0105 (9)*
B3	0.648 (3)	0.7777 (6)	0.8398 (8)	0.0114 (9)*
O1	0.1573 (19)	0.7810 (4)	0.7263 (6)	0.0123 (6)*
O2	0.2686 (18)	0.8155 (4)	0.4182 (5)	0.0116 (6)*
O3	0.5559 (18)	0.9360 (4)	0.7686 (5)	0.0114 (6)*
O4	0.1359 (19)	0.4552 (4)	0.6853 (6)	0.0130 (7)*
O5	0.494 (2)	0.6646 (4)	0.9148 (6)	0.0108 (7)*
O6	0.6998 (19)	0.6626 (4)	0.6658 (6)	0.0107 (6)*
O7	0.2306 (18)	0.0758 (4)	0.6385 (5)	0.0110 (6)*
O8	0.8808 (18)	0.8528 (4)	0.0154 (5)	0.0105 (6)*
O9	0.1488 (18)	0.6352 (4)	0.0152 (5)	0.0111 (6)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
?	?	?	?	?	?	?

Geometric parameters (Å, º)

Ca1—B2	2.974 (17)	O1—O4^v	2.930 (5)
Ca1—O2^i	2.417 (10)	O1—O5	2.433 (13)
Ca1—O4	2.355 (12)	O1—O6^vi	2.647 (16)
Ca1—O5	2.480 (5)	O1—O7^iii	2.371 (5)
Ca1—O5^ii	2.518 (6)	O1—O8^vii	2.990 (13)
Ca1—O6	2.486 (6)	O1—O9^iv	2.367 (6)
Ca1—O6^i	2.434 (4)	O2—O3	2.409 (7)
Ca1—O7	2.339 (6)	O2—O3^viii	2.635 (8)
Ca1—O9^i	2.371 (8)	O2—O4^v	2.733 (12)
B1—B2	2.508 (9)	O2—O7^iii	2.385 (8)
B1—B3	2.511 (19)	O2—O9	2.687 (5)
B1—O1	1.432 (14)	O3—O5	2.400 (5)
B1—O2	1.482 (8)	O3—O6	2.471 (10)
B1—O3	1.472 (17)	O3—O7^iii	2.388 (13)
B1—O5	2.853 (9)	O3—O8^iv	2.402 (11)
B1—O7^iii	1.478 (10)	O4—O4^v	2.784 (8)
B2—B3	2.51 (3)	O4—O5	2.387 (11)
B2—O1	1.426 (10)	O4—O6^i	2.928 (11)
B2—O3	2.854 (15)	O4—O9^iv	2.417 (7)
B2—O4	1.487 (6)	O5—O5^ii	2.867 (5)
B2—O5	1.47 (2)	O5—O6	2.376 (14)
B2—O9^iv	1.495 (16)	O5—O8^iv	2.359 (14)
B3—O1	2.85 (2)	O5—O9^iv	2.376 (17)
B3—O3	1.477 (11)	O6—O8^iv	2.404 (4)
B3—O5	1.401 (16)	O7—O7^ix	2.783 (12)
B3—O6	1.510 (13)	O7—O8^i	2.635 (10)
B3—O8^iv	1.498 (14)	O8—O8^x	2.491 (8)
O1—O2	2.402 (10)	O8—O9^xi	2.505 (12)
O1—O3	2.405 (15)	O9—O9^xii	2.409 (10)
O1—O4	2.405 (5)
B2—Ca1—O2^i	168.4 (3)	O1—O3—O5	60.8 (4)
B2—Ca1—O4	29.6 (3)	O1—O3—O6	98.2 (3)
B2—Ca1—O5	29.5 (4)	O1—O3—O7^iii	59.3 (3)
B2—Ca1—O5^ii	75.8 (3)	O1—O3—O8^iv	118.4 (3)
B2—Ca1—O6	74.2 (4)	O2—O3—O2^viii	83.6 (2)
B2—Ca1—O6^i	93.2 (3)	O2—O3—O5	97.8 (2)
B2—Ca1—O7	105.8 (4)	O2—O3—O6	80.2 (3)
B2—Ca1—O9^i	114.3 (3)	O2—O3—O7^iii	59.6 (3)
O2^i—Ca1—O4	152.45 (17)	O2—O3—O8^iv	139.1 (3)
O2^i—Ca1—O5	145.1 (3)	O2^viii—O3—O5	161.2 (6)
O2^i—Ca1—O5^ii	113.5 (3)	O2^viii—O3—O6	103.8 (4)
O2^i—Ca1—O6	95.0 (3)	O2^viii—O3—O7^iii	77.7 (3)
O2^i—Ca1—O6^i	80.8 (3)	O2^viii—O3—O8^iv	108.4 (5)
O2^i—Ca1—O7	83.1 (3)	O5—O3—O6	58.4 (3)
O2^i—Ca1—O9^i	68.3 (2)	O5—O3—O7^iii	119.3 (6)
O4—Ca1—O5	59.1 (3)	O5—O3—O8^iv	58.8 (3)
O4—Ca1—O5^ii	84.7 (3)	O6—O3—O7^iii	139.6 (3)
O4—Ca1—O6	94.3 (3)	O6—O3—O8^iv	59.1 (3)
O4—Ca1—O6^i	75.4 (3)	O7^iii—O3—O8^iv	159.7 (3)
O4—Ca1—O7	79.6 (3)	Ca1—O4—B2	98.9 (9)
O4—Ca1—O9^i	138.1 (2)	Ca1—O4—O1	116.4 (5)
O5—Ca1—O5^ii	70.00 (15)	Ca1—O4—O1^v	98.1 (3)
O5—Ca1—O6	57.2 (3)	Ca1—O4—O2^v	117.6 (2)
O5—Ca1—O6^i	110.84 (19)	Ca1—O4—O4^v	122.2 (4)
O5—Ca1—O7	130.3 (4)	Ca1—O4—O5	63.1 (4)
O5—Ca1—O9^i	88.2 (2)	Ca1—O4—O6^i	53.5 (3)
O5^ii—Ca1—O6	117.35 (14)	Ca1—O4—O9^iv	112.2 (4)
O5^ii—Ca1—O6^i	154.8 (4)	B2—O4—O1	33.5 (4)
O5^ii—Ca1—O7	80.60 (18)	B2—O4—O1^v	151.5 (5)
O5^ii—Ca1—O9^i	58.1 (4)	B2—O4—O2^v	135.6 (10)
O6—Ca1—O6^i	80.02 (16)	B2—O4—O4^v	101.8 (4)
O6—Ca1—O7	160.67 (14)	B2—O4—O5	35.9 (9)
O6—Ca1—O9^i	87.5 (2)	B2—O4—O6^i	123.4 (9)
O6^i—Ca1—O7	80.69 (17)	B2—O4—O9^iv	36.0 (6)
O6^i—Ca1—O9^i	145.5 (4)	O1—O4—O1^v	118.0 (2)
O7—Ca1—O9^i	109.3 (2)	O1—O4—O2^v	125.9 (5)
B2—B1—B3	60.1 (6)	O1—O4—O4^v	68.31 (18)
B2—B1—O1	28.6 (6)	O1—O4—O5	61.0 (3)
B2—B1—O2	107.6 (3)	O1—O4—O6^i	109.1 (3)
B2—B1—O3	87.6 (5)	O1—O4—O9^iv	58.79 (18)
B2—B1—O5	31.0 (5)	O1^v—O4—O2^v	50.0 (2)
B2—B1—O7^iii	133.8 (9)	O1^v—O4—O4^v	49.70 (14)
B3—B1—O1	87.9 (6)	O1^v—O4—O5	151.7 (5)
B3—B1—O2	101.0 (8)	O1^v—O4—O6^i	53.7 (3)
B3—B1—O3	31.7 (3)	O1^v—O4—O9^iv	147.4 (6)
B3—B1—O5	29.4 (4)	O2^v—O4—O4^v	80.2 (3)
B3—B1—O7^iii	138.1 (6)	O2^v—O4—O5	156.4 (3)
O1—B1—O2	111.0 (5)	O2^v—O4—O6^i	99.3 (2)
O1—B1—O3	111.8 (5)	O2^v—O4—O9^iv	103.0 (4)
O1—B1—O5	58.5 (5)	O4^v—O4—O5	120.6 (2)
O1—B1—O7^iii	109.1 (11)	O4^v—O4—O6^i	70.1 (3)
O2—B1—O3	109.3 (11)	O4^v—O4—O9^iv	116.1 (4)
O2—B1—O5	109.4 (5)	O5—O4—O6^i	98.6 (5)
O2—B1—O7^iii	107.4 (4)	O5—O4—O9^iv	59.3 (4)
O3—B1—O5	57.3 (3)	O6^i—O4—O9^iv	157.6 (5)
O3—B1—O7^iii	108.1 (5)	Ca1—O5—Ca1^ii	110.00 (15)
O5—B1—O7^iii	143.2 (4)	Ca1—O5—B1	112.13 (19)
Ca1—B2—B1	107.5 (7)	Ca1—O5—B2	94.2 (4)
Ca1—B2—B3	66.0 (5)	Ca1—O5—B3	98.1 (6)
Ca1—B2—O1	130.3 (9)	Ca1—O5—O1	110.9 (2)
Ca1—B2—O3	92.6 (6)	Ca1—O5—O3	119.4 (3)
Ca1—B2—O4	51.5 (7)	Ca1—O5—O4	57.9 (2)
Ca1—B2—O5	56.3 (5)	Ca1—O5—O5^ii	55.63 (15)
Ca1—B2—O9^iv	121.3 (5)	Ca1—O5—O6	61.5 (2)
B1—B2—B3	60.0 (5)	Ca1—O5—O8^iv	107.6 (5)
B1—B2—O1	28.7 (7)	Ca1—O5—O9^iv	109.3 (3)
B1—B2—O3	31.0 (4)	Ca1^ii—O5—B1	132.4 (5)
B1—B2—O4	113.4 (4)	Ca1^ii—O5—B2	94.7 (6)
B1—B2—O5	87.6 (7)	Ca1^ii—O5—B3	131.6 (4)
B1—B2—O9^iv	129.0 (7)	Ca1^ii—O5—O1	112.4 (5)
B3—B2—O1	87.9 (8)	Ca1^ii—O5—O3	129.49 (19)
B3—B2—O3	31.1 (3)	Ca1^ii—O5—O4	105.3 (4)
B3—B2—O4	111.8 (11)	Ca1^ii—O5—O5^ii	54.37 (15)
B3—B2—O5	28.1 (4)	Ca1^ii—O5—O6	146.9 (5)
B3—B2—O9^iv	127.0 (7)	Ca1^ii—O5—O8^iv	95.9 (2)
O1—B2—O3	57.3 (7)	Ca1^ii—O5—O9^iv	57.9 (2)
O1—B2—O4	111.3 (6)	B1—O5—B2	61.4 (4)
O1—B2—O5	114.4 (10)	B1—O5—B3	61.6 (7)
O1—B2—O9^iv	108.2 (12)	B1—O5—O1	30.1 (4)
O3—B2—O4	124.8 (9)	B1—O5—O3	31.1 (4)
O3—B2—O5	57.2 (5)	B1—O5—O4	80.0 (3)
O3—B2—O9^iv	126.8 (3)	B1—O5—O5^ii	156.7 (4)
O4—B2—O5	107.7 (12)	B1—O5—O6	75.3 (4)
O4—B2—O9^iv	108.3 (9)	B1—O5—O8^iv	91.7 (3)
O5—B2—O9^iv	106.6 (7)	B1—O5—O9^iv	87.7 (5)
B1—B3—B2	59.9 (5)	B2—O5—B3	122.3 (7)
B1—B3—O1	30.2 (3)	B2—O5—O1	32.2 (3)
B1—B3—O3	31.6 (5)	B2—O5—O3	91.8 (5)
B1—B3—O5	88.9 (9)	B2—O5—O4	36.4 (4)
B1—B3—O6	103.4 (5)	B2—O5—O5^ii	97.8 (5)
B1—B3—O8^iv	137.5 (4)	B2—O5—O6	117.2 (5)
B2—B3—O1	30.1 (3)	B2—O5—O8^iv	150.7 (4)
B2—B3—O3	87.3 (9)	B2—O5—O9^iv	37.1 (5)
B2—B3—O5	29.6 (6)	B3—O5—O1	91.8 (6)
B2—B3—O6	108.3 (6)	B3—O5—O3	34.5 (6)
B2—B3—O8^iv	133.7 (6)	B3—O5—O4	123.0 (4)
O1—B3—O3	57.7 (7)	B3—O5—O5^ii	134.9 (9)
O1—B3—O5	58.7 (7)	B3—O5—O6	36.8 (4)
O1—B3—O6	111.9 (6)	B3—O5—O8^iv	36.9 (5)
O1—B3—O8^iv	142.0 (7)	B3—O5—O9^iv	145.1 (7)
O3—B3—O5	113.0 (13)	O1—O5—O3	59.7 (3)
O3—B3—O6	111.6 (5)	O1—O5—O4	59.9 (3)
O3—B3—O8^iv	107.7 (4)	O1—O5—O5^ii	130.0 (5)
O5—B3—O6	109.3 (5)	O1—O5—O6	100.0 (3)
O5—B3—O8^iv	108.8 (5)	O1—O5—O8^iv	119.0 (3)
O6—B3—O8^iv	106.1 (12)	O1—O5—O9^iv	58.9 (4)
B1—O1—B2	122.7 (13)	O3—O5—O4	109.1 (3)
B1—O1—B3	61.9 (7)	O3—O5—O5^ii	169.4 (7)
B1—O1—O2	35.2 (3)	O3—O5—O6	62.3 (3)
B1—O1—O3	34.6 (5)	O3—O5—O8^iv	60.6 (3)
B1—O1—O4	121.7 (7)	O3—O5—O9^iv	111.0 (5)
B1—O1—O4^v	94.8 (3)	O4—O5—O5^ii	76.8 (2)
B1—O1—O5	91.4 (8)	O4—O5—O6	96.4 (3)
B1—O1—O6^vi	138.0 (6)	O4—O5—O8^iv	157.3 (4)
B1—O1—O7^iii	36.1 (6)	O4—O5—O9^iv	61.0 (4)
B1—O1—O8^vii	133.6 (5)	O5^ii—O5—O6	108.9 (4)
B1—O1—O9^iv	145.6 (7)	O5^ii—O5—O8^iv	110.6 (4)
B2—O1—B3	62.0 (9)	O5^ii—O5—O9^iv	79.6 (3)
B2—O1—O2	115.3 (9)	O6—O5—O8^iv	61.0 (4)
B2—O1—O3	92.7 (10)	O6—O5—O9^iv	154.1 (4)
B2—O1—O4	35.2 (3)	O8^iv—O5—O9^iv	140.3 (3)
B2—O1—O4^v	97.1 (3)	Ca1—O6—Ca1^i	99.98 (19)
B2—O1—O5	33.3 (8)	Ca1—O6—B3	94.8 (5)
B2—O1—O6^vi	96.5 (9)	Ca1—O6—O1^xi	128.3 (3)
B2—O1—O7^iii	151.7 (9)	Ca1—O6—O3	116.4 (5)
B2—O1—O8^vii	91.0 (8)	Ca1—O6—O4^i	101.77 (17)
B2—O1—O9^iv	36.9 (7)	Ca1—O6—O5	61.3 (2)
B3—O1—O2	73.2 (4)	Ca1—O6—O8^iv	106.0 (2)
B3—O1—O3	31.3 (2)	Ca1^i—O6—B3	125.4 (6)
B3—O1—O4	79.1 (4)	Ca1^i—O6—O1^xi	104.2 (3)
B3—O1—O4^v	113.7 (4)	Ca1^i—O6—O3	94.4 (3)
B3—O1—O5	29.5 (3)	Ca1^i—O6—O4^i	51.1 (2)
B3—O1—O6^vi	158.2 (2)	Ca1^i—O6—O5	123.5 (5)
B3—O1—O7^iii	91.3 (4)	Ca1^i—O6—O8^iv	149.1 (2)
B3—O1—O8^vii	128.0 (2)	B3—O6—O1^xi	106.6 (6)
B3—O1—O9^iv	87.4 (4)	B3—O6—O3	33.8 (3)
O2—O1—O3	60.2 (3)	B3—O6—O4^i	163.4 (4)
O2—O1—O4	95.4 (3)	B3—O6—O5	33.8 (4)
O2—O1—O4^v	60.7 (2)	B3—O6—O8^iv	36.8 (6)
O2—O1—O5	97.1 (5)	O1^xi—O6—O3	106.5 (3)
O2—O1—O6^vi	117.4 (3)	O1^xi—O6—O4^i	63.2 (3)
O2—O1—O7^iii	60.0 (2)	O1^xi—O6—O5	129.9 (3)
O2—O1—O8^vii	153.1 (4)	O1^xi—O6—O8^iv	72.4 (3)
O2—O1—O9^iv	152.2 (5)	O3—O6—O4^i	133.2 (2)
O3—O1—O4	108.3 (5)	O3—O6—O5	59.3 (3)
O3—O1—O4^v	118.3 (4)	O3—O6—O8^iv	59.0 (3)
O3—O1—O5	59.5 (3)	O4^i—O6—O5	162.4 (2)
O3—O1—O6^vi	170.4 (3)	O4^i—O6—O8^iv	135.6 (5)
O3—O1—O7^iii	60.0 (3)	O5—O6—O8^iv	59.1 (3)
O3—O1—O8^vii	127.4 (2)	Ca1—O7—B1^xiii	124.7 (8)
O3—O1—O9^iv	111.1 (4)	Ca1—O7—O1^xiii	146.8 (4)
O4—O1—O4^v	61.98 (16)	Ca1—O7—O2^xiii	121.5 (5)
O4—O1—O5	59.1 (3)	Ca1—O7—O3^xiii	90.5 (4)
O4—O1—O6^vi	80.9 (4)	Ca1—O7—O7^ix	134.1 (2)
O4—O1—O7^iii	155.3 (4)	Ca1—O7—O8^i	93.31 (17)
O4—O1—O8^vii	104.3 (3)	B1^xiii—O7—O1^xiii	34.8 (6)
O4—O1—O9^iv	60.85 (18)	B1^xiii—O7—O2^xiii	36.4 (3)
O4^v—O1—O5	113.6 (3)	B1^xiii—O7—O3^xiii	35.9 (5)
O4^v—O1—O6^vi	63.1 (3)	B1^xiii—O7—O7^ix	95.1 (5)
O4^v—O1—O7^iii	102.62 (17)	B1^xiii—O7—O8^i	106.0 (4)
O4^v—O1—O8^vii	113.1 (4)	O1^xiii—O7—O2^xiii	60.7 (2)
O4^v—O1—O9^iv	112.5 (2)	O1^xiii—O7—O3^xiii	60.7 (3)
O5—O1—O6^vi	129.5 (3)	O1^xiii—O7—O7^ix	78.9 (3)
O5—O1—O7^iii	118.6 (5)	O1^xiii—O7—O8^i	77.6 (3)
O5—O1—O8^vii	108.6 (3)	O2^xiii—O7—O3^xiii	60.6 (3)
O5—O1—O9^iv	59.3 (4)	O2^xiii—O7—O7^ix	76.2 (3)
O6^vi—O1—O7^iii	110.5 (4)	O2^xiii—O7—O8^i	138.2 (2)
O6^vi—O1—O8^vii	50.0 (2)	O3^xiii—O7—O7^ix	130.87 (19)
O6^vi—O1—O9^iv	75.4 (4)	O3^xiii—O7—O8^i	100.3 (3)
O7^iii—O1—O8^vii	99.6 (3)	O7^ix—O7—O8^i	96.7 (4)
O7^iii—O1—O9^iv	142.1 (2)	B3^xiv—O8—O1^xv	92.5 (6)
O8^vii—O1—O9^iv	54.3 (3)	B3^xiv—O8—O3^xiv	35.9 (3)
Ca1^i—O2—B1	128.9 (7)	B3^xiv—O8—O5^xiv	34.2 (5)
Ca1^i—O2—O1	124.9 (3)	B3^xiv—O8—O6^xiv	37.1 (6)
Ca1^i—O2—O3	96.5 (4)	B3^xiv—O8—O7^i	105.0 (8)
Ca1^i—O2—O3^viii	83.2 (3)	B3^xiv—O8—O8^x	115.2 (3)
Ca1^i—O2—O4^v	98.5 (2)	B3^xiv—O8—O9^xi	110.2 (5)
Ca1^i—O2—O7^iii	151.5 (5)	O1^xv—O8—O3^xiv	98.5 (3)
Ca1^i—O2—O9	55.1 (3)	O1^xv—O8—O5^xiv	116.2 (2)
B1—O2—O1	33.8 (5)	O1^xv—O8—O6^xiv	57.6 (3)
B1—O2—O3	35.2 (7)	O1^xv—O8—O7^i	161.8 (4)
B1—O2—O3^viii	110.5 (4)	O1^xv—O8—O8^x	69.3 (3)
B1—O2—O4^v	102.0 (7)	O1^xv—O8—O9^xi	50.1 (2)
B1—O2—O7^iii	36.3 (4)	O3^xiv—O8—O5^xiv	60.5 (3)
B1—O2—O9	171.7 (8)	O3^xiv—O8—O6^xiv	61.9 (3)
O1—O2—O3	60.0 (3)	O3^xiv—O8—O7^i	98.8 (5)
O1—O2—O3^viii	142.69 (19)	O3^xiv—O8—O8^x	84.2 (3)
O1—O2—O4^v	69.3 (3)	O3^xiv—O8—O9^xi	138.8 (2)
O1—O2—O7^iii	59.4 (2)	O5^xiv—O8—O6^xiv	59.8 (3)
O1—O2—O9	138.2 (3)	O5^xiv—O8—O7^i	77.8 (4)
O3—O2—O3^viii	96.4 (3)	O5^xiv—O8—O8^x	144.6 (4)
O3—O2—O4^v	126.3 (3)	O5^xiv—O8—O9^xi	105.6 (3)
O3—O2—O7^iii	59.8 (3)	O6^xiv—O8—O7^i	137.7 (5)
O3—O2—O9	151.0 (6)	O6^xiv—O8—O8^x	108.0 (3)
O3^viii—O2—O4^v	136.5 (3)	O6^xiv—O8—O9^xi	77.5 (3)
O3^viii—O2—O7^iii	84.2 (2)	O7^i—O8—O8^x	106.7 (2)
O3^viii—O2—O9	76.47 (19)	O7^i—O8—O9^xi	116.9 (2)
O4^v—O2—O7^iii	108.3 (5)	O8^x—O8—O9^xi	103.3 (5)
O4^v—O2—O9	69.7 (3)	Ca1^i—O9—B2^xiv	100.1 (9)
O7^iii—O2—O9	144.4 (3)	Ca1^i—O9—O1^xiv	120.6 (5)
B1—O3—B2	61.4 (5)	Ca1^i—O9—O2	56.7 (2)
B1—O3—B3	116.7 (6)	Ca1^i—O9—O4^xiv	109.1 (5)
B1—O3—O1	33.6 (4)	Ca1^i—O9—O5^xiv	64.1 (3)
B1—O3—O2	35.5 (5)	Ca1^i—O9—O8^vi	127.72 (17)
B1—O3—O2^viii	99.9 (4)	Ca1^i—O9—O9^xii	109.4 (2)
B1—O3—O5	91.7 (5)	B2^xiv—O9—O1^xiv	34.9 (5)
B1—O3—O6	106.6 (4)	B2^xiv—O9—O2	139.3 (6)
B1—O3—O7^iii	36.0 (3)	B2^xiv—O9—O4^xiv	35.7 (3)
B1—O3—O8^iv	150.5 (4)	B2^xiv—O9—O5^xiv	36.3 (7)
B2—O3—B3	61.6 (8)	B2^xiv—O9—O8^vi	110.4 (6)
B2—O3—O1	29.9 (4)	B2^xiv—O9—O9^xii	115.2 (4)
B2—O3—O2	76.5 (3)	O1^xiv—O9—O2	124.20 (16)
B2—O3—O2^viii	159.8 (3)	O1^xiv—O9—O4^xiv	60.36 (18)
B2—O3—O5	31.0 (4)	O1^xiv—O9—O5^xiv	61.7 (4)
B2—O3—O6	76.6 (4)	O1^xiv—O9—O8^vi	75.7 (3)
B2—O3—O7^iii	89.0 (5)	O1^xiv—O9—O9^xii	123.1 (3)
B2—O3—O8^iv	89.4 (4)	O2—O9—O4^xiv	165.8 (5)
B3—O3—O1	91.0 (7)	O2—O9—O5^xiv	109.1 (4)
B3—O3—O2	105.7 (3)	O2—O9—O8^vi	72.9 (3)
B3—O3—O2^viii	129.1 (9)	O2—O9—O9^xii	104.5 (3)
B3—O3—O5	32.5 (7)	O4^xiv—O9—O5^xiv	59.7 (3)
B3—O3—O6	34.6 (4)	O4^xiv—O9—O8^vi	120.6 (3)
B3—O3—O7^iii	150.3 (8)	O4^xiv—O9—O9^xii	79.8 (3)
B3—O3—O8^iv	36.5 (4)	O5^xiv—O9—O8^vi	129.5 (3)
O1—O3—O2	59.9 (3)	O5^xiv—O9—O9^xii	130.1 (3)
O1—O3—O2^viii	133.1 (4)	O8^vi—O9—O9^xii	94.9 (5)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y+1, −z+2; (iii) x, y+1, z; (iv) x, y, z+1; (v) −x, −y+1, −z+1; (vi) x−1, y, z; (vii) x−1, y, z+1; (viii) −x+1, −y+2, −z+1; (ix) −x, −y, −z+1; (x) −x+2, −y+2, −z; (xi) x+1, y, z; (xii) −x, −y+1, −z; (xiii) x, y−1, z; (xiv) x, y, z−1; (xv) x+1, y, z−1.

(II_7.38GPa)

Crystal data

H7B3CaO9	Z = 2
Mr = 223.6	F(000) = 214
Triclinic, P1	Dx = 2.573 Mg m^−3
Hall symbol: -P 1	Synchrotron radiation, λ = 0.41066 Å
a = 6.050 (3) Å	Cell parameters from 603 reflections
b = 7.4908 (2) Å	θ = 3.6–20.1°
c = 6.7136 (3) Å	µ = 0.26 mm^−1
α = 97.629 (3)°	T = 293 K
β = 107.773 (14)°	Prismatic habit, colourless
γ = 100.211 (11)°	0.02 × 0.01 × 0.01 mm
V = 279.42 (14) Å^3

Data collection

Beamline diffractometer	374 reflections with I > 3σ(I)
Radiation source: ESRF: Synchrotron radiation, undulator, IVU20c	Rint = 0.011
Silicon monochromator	θmax = 20.1°, θmin = 2.7°
ω scans	h = −3→4
603 measured reflections	k = −12→12
403 independent reflections	l = −11→10

Refinement

Refinement on F	0 constraints
R[F^2 > 2σ(F^2)] = 0.043	H-atom parameters not defined
wR(F^2) = 0.056	Weighting scheme based on measured s.u.'s w = 1/(σ^2(F) + 0.0001F^2)
S = 3.32	(Δ/σ)max = 0.025
403 reflections	Δρmax = 0.31 e Å^−3
53 parameters	Δρmin = −0.30 e Å^−3
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.4926 (6)	0.36399 (12)	0.71337 (17)	0.0102 (3)*
B1	0.305 (3)	0.8990 (7)	0.6421 (9)	0.0085 (9)*
B2	0.237 (4)	0.6393 (8)	0.8317 (11)	0.0098 (10)*
B3	0.648 (3)	0.7786 (7)	0.8414 (9)	0.0105 (10)*
O1	0.155 (2)	0.7819 (5)	0.7266 (6)	0.0113 (7)*
O2	0.269 (2)	0.8153 (4)	0.4175 (6)	0.0105 (7)*
O3	0.557 (2)	0.9376 (4)	0.7706 (6)	0.0114 (7)*
O4	0.133 (2)	0.4551 (5)	0.6840 (6)	0.0124 (7)*
O5	0.497 (2)	0.6647 (5)	0.9158 (7)	0.0112 (7)*
O6	0.700 (2)	0.6632 (4)	0.6663 (6)	0.0106 (7)*
O7	0.2276 (19)	0.0764 (4)	0.6367 (6)	0.0099 (7)*
O8	0.883 (2)	0.8533 (4)	0.0176 (6)	0.0105 (7)*
O9	0.151 (2)	0.6357 (4)	0.0170 (6)	0.0104 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
?	?	?	?	?	?	?

Geometric parameters (Å, º)

Ca1—B2	2.952 (19)	O1—O4^v	2.909 (6)
Ca1—B2^i	2.998 (9)	O1—O5	2.447 (15)
Ca1—O2^ii	2.411 (11)	O1—O6^vi	2.626 (17)
Ca1—O4	2.352 (13)	O1—O7^iii	2.365 (5)
Ca1—O5	2.463 (6)	O1—O8^vii	2.968 (15)
Ca1—O5^i	2.509 (6)	O1—O9^iv	2.364 (6)
Ca1—O6	2.475 (6)	O2—O3	2.416 (8)
Ca1—O6^ii	2.421 (4)	O2—O3^viii	2.622 (9)
Ca1—O7	2.336 (6)	O2—O4^v	2.712 (13)
Ca1—O9^ii	2.353 (9)	O2—O7^iii	2.384 (9)
B1—B2	2.503 (11)	O2—O9	2.660 (6)
B1—B3	2.49 (2)	O3—O5	2.397 (6)
B1—O1	1.440 (16)	O3—O6	2.466 (11)
B1—O2	1.488 (9)	O3—O7^iii	2.398 (14)
B1—O3	1.460 (19)	O3—O8^iv	2.401 (12)
B1—O5	2.843 (10)	O4—O4^v	2.748 (8)
B1—O7^iii	1.485 (12)	O4—O5	2.399 (12)
B2—B3	2.49 (3)	O4—O6^ii	2.924 (13)
B2—O1	1.436 (12)	O4—O7	2.987 (8)
B2—O3	2.846 (17)	O4—O9^iv	2.416 (8)
B2—O4	1.493 (6)	O5—O5^i	2.849 (6)
B2—O5	1.46 (3)	O5—O6	2.361 (15)
B2—O9^iv	1.490 (18)	O5—O8^iv	2.351 (16)
B3—O1	2.85 (2)	O5—O9^iv	2.371 (18)
B3—O3	1.472 (11)	O6—O8^iv	2.403 (5)
B3—O5	1.389 (17)	O7—O7^ix	2.738 (12)
B3—O6	1.511 (14)	O7—O8^ii	2.619 (11)
B3—O8^iv	1.502 (15)	O8—O8^x	2.475 (9)
O1—O2	2.406 (11)	O8—O9^xi	2.496 (14)
O1—O3	2.413 (16)	O9—O9^xii	2.415 (10)
O1—O4	2.402 (6)
B2—Ca1—B2^i	93.5 (4)	O1—O3—O5	61.2 (4)
B2—Ca1—O2^ii	168.7 (3)	O1—O3—O6	98.1 (3)
B2—Ca1—O4	30.1 (3)	O1—O3—O7^iii	58.9 (4)
B2—Ca1—O5	29.6 (4)	O1—O3—O8^iv	118.6 (3)
B2—Ca1—O5^i	75.5 (3)	O2—O3—O2^viii	83.5 (2)
B2—Ca1—O6	74.2 (4)	O2—O3—O5	97.6 (3)
B2—Ca1—O6^ii	93.8 (3)	O2—O3—O6	79.7 (3)
B2—Ca1—O7	105.7 (4)	O2—O3—O7^iii	59.4 (3)
B2—Ca1—O9^ii	114.1 (3)	O2—O3—O8^iv	138.7 (4)
B2^i—Ca1—O2^ii	92.1 (4)	O2^viii—O3—O5	160.8 (7)
B2^i—Ca1—O4	111.0 (5)	O2^viii—O3—O6	103.6 (5)
B2^i—Ca1—O5	75.3 (3)	O2^viii—O3—O7^iii	77.8 (3)
B2^i—Ca1—O5^i	29.1 (6)	O2^viii—O3—O8^iv	108.5 (5)
B2^i—Ca1—O6	101.9 (3)	O5—O3—O6	58.1 (3)
B2^i—Ca1—O6^ii	172.6 (4)	O5—O3—O7^iii	119.3 (6)
B2^i—Ca1—O7	97.4 (2)	O5—O3—O8^iv	58.7 (4)
B2^i—Ca1—O9^ii	29.3 (5)	O6—O3—O7^iii	138.9 (3)
O2^ii—Ca1—O4	152.48 (19)	O6—O3—O8^iv	59.2 (3)
O2^ii—Ca1—O5	144.6 (4)	O7^iii—O3—O8^iv	160.3 (4)
O2^ii—Ca1—O5^i	113.3 (3)	Ca1—O4—B2	97.8 (11)
O2^ii—Ca1—O6	95.0 (3)	Ca1—O4—O1	116.2 (5)
O2^ii—Ca1—O6^ii	80.7 (3)	Ca1—O4—O1^v	97.7 (3)
O2^ii—Ca1—O7	83.3 (3)	Ca1—O4—O2^v	117.7 (3)
O2^ii—Ca1—O9^ii	67.9 (2)	Ca1—O4—O4^v	121.9 (4)
O4—Ca1—O5	59.7 (3)	Ca1—O4—O5	62.5 (4)
O4—Ca1—O5^i	84.6 (3)	Ca1—O4—O6^ii	53.3 (3)
O4—Ca1—O6	94.6 (3)	Ca1—O4—O7	50.2 (3)
O4—Ca1—O6^ii	75.6 (3)	Ca1—O4—O9^iv	111.5 (4)
O4—Ca1—O7	79.2 (3)	B2—O4—O1	34.1 (5)
O4—Ca1—O9^ii	138.3 (2)	B2—O4—O1^v	152.7 (5)
O5—Ca1—O5^i	69.89 (17)	B2—O4—O2^v	136.1 (11)
O5—Ca1—O6	57.1 (3)	B2—O4—O4^v	102.5 (5)
O5—Ca1—O6^ii	111.5 (2)	B2—O4—O5	35.3 (10)
O5—Ca1—O7	130.4 (4)	B2—O4—O6^ii	122.9 (10)
O5—Ca1—O9^ii	88.0 (3)	B2—O4—O7	139.1 (8)
O5^i—Ca1—O6	117.41 (16)	B2—O4—O9^iv	35.9 (7)
O5^i—Ca1—O6^ii	154.7 (4)	O1—O4—O1^v	118.6 (3)
O5^i—Ca1—O7	80.5 (2)	O1—O4—O2^v	126.0 (6)
O5^i—Ca1—O9^ii	58.3 (4)	O1—O4—O4^v	68.4 (2)
O6—Ca1—O6^ii	80.29 (18)	O1—O4—O5	61.3 (3)
O6—Ca1—O7	160.65 (16)	O1—O4—O6^ii	109.3 (3)
O6—Ca1—O9^ii	87.5 (3)	O1—O4—O7	166.3 (6)
O6^ii—Ca1—O7	80.42 (18)	O1—O4—O9^iv	58.8 (2)
O6^ii—Ca1—O9^ii	145.2 (4)	O1^v—O4—O2^v	50.5 (2)
O7—Ca1—O9^ii	109.4 (2)	O1^v—O4—O4^v	50.15 (15)
B2—B1—B3	59.9 (6)	O1^v—O4—O5	151.2 (6)
B2—B1—O1	29.4 (7)	O1^v—O4—O6^ii	53.5 (3)
B2—B1—O2	107.5 (3)	O1^v—O4—O7	66.84 (19)
B2—B1—O3	87.7 (6)	O1^v—O4—O9^iv	148.6 (6)
B2—B1—O5	30.9 (6)	O2^v—O4—O4^v	80.9 (3)
B2—B1—O7^iii	133.6 (11)	O2^v—O4—O5	156.0 (3)
B3—B1—O1	88.6 (6)	O2^v—O4—O6^ii	99.6 (2)
B3—B1—O2	101.4 (9)	O2^v—O4—O7	67.5 (3)
B3—B1—O3	32.0 (3)	O2^v—O4—O9^iv	103.2 (5)
B3—B1—O5	29.2 (4)	O4^v—O4—O5	120.5 (3)
B3—B1—O7^iii	139.3 (6)	O4^v—O4—O6^ii	70.1 (3)
O1—B1—O2	110.5 (6)	O4^v—O4—O7	115.64 (18)
O1—B1—O3	112.6 (6)	O4^v—O4—O9^iv	116.7 (4)
O1—B1—O5	59.4 (6)	O5—O4—O6^ii	98.2 (5)
O1—B1—O7^iii	107.9 (12)	O5—O4—O7	107.5 (5)
O2—B1—O3	110.0 (13)	O5—O4—O9^iv	59.0 (4)
O2—B1—O5	109.4 (6)	O6^ii—O4—O7	62.6 (2)
O2—B1—O7^iii	106.6 (5)	O6^ii—O4—O9^iv	156.9 (5)
O3—B1—O5	57.4 (4)	O7—O4—O9^iv	124.1 (2)
O3—B1—O7^iii	109.0 (6)	Ca1—O5—Ca1^i	110.11 (16)
O5—B1—O7^iii	144.0 (4)	Ca1—O5—B1	111.9 (2)
Ca1—B2—Ca1^i	86.5 (4)	Ca1—O5—B2	94.0 (4)
Ca1—B2—B1	107.3 (8)	Ca1—O5—B3	98.7 (7)
Ca1—B2—B3	66.4 (6)	Ca1—O5—O1	110.5 (3)
Ca1—B2—O1	130.5 (9)	Ca1—O5—O3	119.6 (4)
Ca1—B2—O3	92.8 (7)	Ca1—O5—O4	57.8 (3)
Ca1—B2—O4	52.1 (8)	Ca1—O5—O5^i	55.81 (17)
Ca1—B2—O5	56.4 (6)	Ca1—O5—O6	61.7 (3)
Ca1—B2—O9^iv	121.5 (5)	Ca1—O5—O8^iv	108.0 (6)
Ca1^i—B2—B1	125.6 (5)	Ca1—O5—O9^iv	109.2 (3)
Ca1^i—B2—B3	81.0 (5)	Ca1^i—O5—B1	132.3 (5)
Ca1^i—B2—O1	132.8 (4)	Ca1^i—O5—B2	94.3 (7)
Ca1^i—B2—O3	98.7 (5)	Ca1^i—O5—B3	131.8 (5)
Ca1^i—B2—O4	116.4 (5)	Ca1^i—O5—O1	112.0 (6)
Ca1^i—B2—O5	56.6 (4)	Ca1^i—O5—O3	129.3 (2)
Ca1^i—B2—O9^iv	50.6 (5)	Ca1^i—O5—O4	105.1 (4)
B1—B2—B3	59.8 (6)	Ca1^i—O5—O5^i	54.29 (17)
B1—B2—O1	29.6 (8)	Ca1^i—O5—O6	147.3 (6)
B1—B2—O3	30.8 (4)	Ca1^i—O5—O8^iv	96.0 (3)
B1—B2—O4	113.0 (5)	Ca1^i—O5—O9^iv	57.6 (3)
B1—B2—O5	87.5 (8)	B1—O5—B2	61.6 (5)
B1—B2—O9^iv	129.1 (7)	B1—O5—B3	61.1 (7)
B3—B2—O1	88.6 (9)	B1—O5—O1	30.4 (4)
B3—B2—O3	31.1 (3)	B1—O5—O3	30.9 (4)
B3—B2—O4	112.6 (12)	B1—O5—O4	79.8 (4)
B3—B2—O5	28.2 (5)	B1—O5—O5^i	156.4 (5)
B3—B2—O9^iv	127.0 (7)	B1—O5—O6	75.1 (4)
O1—B2—O3	58.0 (7)	B1—O5—O8^iv	91.6 (4)
O1—B2—O4	110.2 (7)	B1—O5—O9^iv	87.8 (5)
O1—B2—O5	115.2 (11)	B2—O5—B3	122.0 (8)
O1—B2—O9^iv	107.8 (14)	B2—O5—O1	32.1 (4)
O3—B2—O4	125.1 (10)	B2—O5—O3	91.7 (5)
O3—B2—O5	57.3 (6)	B2—O5—O4	36.2 (4)
O3—B2—O9^iv	126.7 (4)	B2—O5—O5^i	97.3 (5)
O4—B2—O5	108.5 (13)	B2—O5—O6	117.2 (6)
O4—B2—O9^iv	108.2 (10)	B2—O5—O8^iv	150.6 (4)
O5—B2—O9^iv	106.8 (7)	B2—O5—O9^iv	37.0 (6)
B1—B3—B2	60.3 (6)	B3—O5—O1	91.6 (7)
B1—B3—O1	30.4 (4)	B3—O5—O3	34.2 (7)
B1—B3—O3	31.8 (5)	B3—O5—O4	123.0 (4)
B1—B3—O5	89.6 (10)	B3—O5—O5^i	135.9 (10)
B1—B3—O6	103.2 (5)	B3—O5—O6	37.2 (5)
B1—B3—O8^iv	137.7 (4)	B3—O5—O8^iv	37.2 (5)
B2—B3—O1	30.3 (3)	B3—O5—O9^iv	144.6 (8)
B2—B3—O3	87.7 (10)	O1—O5—O3	59.8 (4)
B2—B3—O5	29.8 (6)	O1—O5—O4	59.4 (3)
B2—B3—O6	108.3 (6)	O1—O5—O5^i	129.3 (6)
B2—B3—O8^iv	133.8 (7)	O1—O5—O6	100.0 (3)
O1—B3—O3	58.0 (8)	O1—O5—O8^iv	119.2 (3)
O1—B3—O5	59.3 (8)	O1—O5—O9^iv	58.7 (4)
O1—B3—O6	111.8 (7)	O3—O5—O4	108.9 (3)
O1—B3—O8^iv	142.4 (8)	O3—O5—O5^i	170.1 (8)
O3—B3—O5	113.8 (14)	O3—O5—O6	62.4 (3)
O3—B3—O6	111.5 (5)	O3—O5—O8^iv	60.7 (4)
O3—B3—O8^iv	107.6 (5)	O3—O5—O9^iv	110.7 (5)
O5—B3—O6	109.0 (5)	O4—O5—O5^i	76.7 (3)
O5—B3—O8^iv	108.8 (6)	O4—O5—O6	96.4 (3)
O6—B3—O8^iv	105.8 (13)	O4—O5—O8^iv	157.6 (5)
B1—O1—B2	121.0 (14)	O4—O5—O9^iv	60.9 (4)
B1—O1—B3	61.0 (7)	O5^i—O5—O6	109.3 (5)
B1—O1—O2	35.4 (3)	O5^i—O5—O8^iv	111.1 (5)
B1—O1—O3	34.0 (6)	O5^i—O5—O9^iv	79.1 (4)
B1—O1—O4	121.1 (8)	O6—O5—O8^iv	61.3 (4)
B1—O1—O4^v	95.0 (3)	O6—O5—O9^iv	154.0 (4)
B1—O1—O5	90.2 (8)	O8^iv—O5—O9^iv	140.0 (3)
B1—O1—O6^vi	139.0 (7)	Ca1—O6—Ca1^ii	99.7 (2)
B1—O1—O7^iii	36.7 (6)	Ca1—O6—B3	94.8 (6)
B1—O1—O8^vii	134.0 (5)	Ca1—O6—O1^xi	128.6 (4)
B1—O1—O9^iv	144.2 (8)	Ca1—O6—O3	116.4 (5)
B2—O1—B3	61.2 (10)	Ca1—O6—O4^ii	101.79 (18)
B2—O1—O2	114.5 (10)	Ca1—O6—O5	61.2 (2)
B2—O1—O3	91.8 (10)	Ca1—O6—O8^iv	106.0 (2)
B2—O1—O4	35.7 (3)	Ca1^ii—O6—B3	125.8 (7)
B2—O1—O4^v	97.1 (3)	Ca1^ii—O6—O1^xi	104.0 (4)
B2—O1—O5	32.8 (9)	Ca1^ii—O6—O3	94.9 (3)
B2—O1—O6^vi	97.1 (10)	Ca1^ii—O6—O4^ii	51.1 (2)
B2—O1—O7^iii	151.0 (11)	Ca1^ii—O6—O5	124.0 (6)
B2—O1—O8^vii	91.2 (9)	Ca1^ii—O6—O8^iv	149.5 (2)
B2—O1—O9^iv	36.9 (8)	B3—O6—O1^xi	106.6 (7)
B3—O1—O2	73.0 (4)	B3—O6—O3	33.7 (3)
B3—O1—O3	31.1 (2)	B3—O6—O4^ii	163.4 (5)
B3—O1—O4	79.2 (4)	B3—O6—O5	33.8 (5)
B3—O1—O4^v	113.2 (4)	B3—O6—O8^iv	37.0 (7)
B3—O1—O5	29.2 (3)	O1^xi—O6—O3	106.2 (3)
B3—O1—O6^vi	158.1 (2)	O1^xi—O6—O4^ii	62.9 (3)
B3—O1—O7^iii	91.3 (4)	O1^xi—O6—O5	129.8 (3)
B3—O1—O8^vii	127.5 (3)	O1^xi—O6—O8^iv	72.2 (4)
B3—O1—O9^iv	86.7 (4)	O3—O6—O4^ii	133.4 (2)
O2—O1—O3	60.2 (3)	O3—O6—O5	59.5 (3)
O2—O1—O4	94.9 (3)	O3—O6—O8^iv	59.1 (3)
O2—O1—O4^v	60.5 (3)	O4^ii—O6—O5	162.5 (3)
O2—O1—O5	96.5 (6)	O4^ii—O6—O8^iv	135.1 (6)
O2—O1—O6^vi	117.7 (3)	O5—O6—O8^iv	59.2 (4)
O2—O1—O7^iii	59.9 (2)	Ca1—O7—B1^xiii	123.4 (9)
O2—O1—O8^vii	153.9 (4)	Ca1—O7—O1^xiii	146.4 (4)
O2—O1—O9^iv	151.4 (5)	Ca1—O7—O2^xiii	121.1 (5)
O3—O1—O4	108.2 (6)	Ca1—O7—O3^xiii	89.9 (4)
O3—O1—O4^v	118.0 (4)	Ca1—O7—O4	50.7 (2)
O3—O1—O5	59.1 (4)	Ca1—O7—O7^ix	134.9 (2)
O3—O1—O6^vi	170.7 (3)	Ca1—O7—O8^ii	93.45 (18)
O3—O1—O7^iii	60.2 (4)	B1^xiii—O7—O1^xiii	35.4 (7)
O3—O1—O8^vii	127.1 (2)	B1^xiii—O7—O2^xiii	36.7 (3)
O3—O1—O9^iv	110.4 (4)	B1^xiii—O7—O3^xiii	35.2 (6)
O4—O1—O4^v	61.45 (18)	B1^xiii—O7—O4	171.7 (5)
O4—O1—O5	59.3 (3)	B1^xiii—O7—O7^ix	95.8 (6)
O4—O1—O6^vi	80.7 (4)	B1^xiii—O7—O8^ii	105.6 (5)
O4—O1—O7^iii	154.8 (5)	O1^xiii—O7—O2^xiii	60.9 (3)
O4—O1—O8^vii	104.3 (4)	O1^xiii—O7—O3^xiii	60.9 (4)
O4—O1—O9^iv	60.9 (2)	O1^xiii—O7—O4	145.3 (5)
O4^v—O1—O5	112.9 (3)	O1^xiii—O7—O7^ix	78.7 (3)
O4^v—O1—O6^vi	63.5 (3)	O1^xiii—O7—O8^ii	77.1 (3)
O4^v—O1—O7^iii	102.45 (19)	O2^xiii—O7—O3^xiii	60.7 (3)
O4^v—O1—O8^vii	114.0 (5)	O2^xiii—O7—O4	149.3 (2)
O4^v—O1—O9^iv	112.7 (2)	O2^xiii—O7—O7^ix	76.2 (3)
O5—O1—O6^vi	129.6 (3)	O2^xiii—O7—O8^ii	138.0 (2)
O5—O1—O7^iii	118.6 (5)	O3^xiii—O7—O4	137.0 (3)
O5—O1—O8^vii	108.4 (3)	O3^xiii—O7—O7^ix	130.9 (2)
O5—O1—O9^iv	59.0 (4)	O3^xiii—O7—O8^ii	99.8 (3)
O6^vi—O1—O7^iii	110.6 (5)	O4—O7—O7^ix	92.1 (4)
O6^vi—O1—O8^vii	50.4 (3)	O4—O7—O8^ii	70.8 (2)
O6^vi—O1—O9^iv	75.8 (4)	O7^ix—O7—O8^ii	96.7 (5)
O7^iii—O1—O8^vii	100.0 (4)	B3^xiv—O8—O1^xv	92.4 (7)
O7^iii—O1—O9^iv	142.5 (2)	B3^xiv—O8—O3^xiv	35.8 (3)
O8^vii—O1—O9^iv	54.4 (3)	B3^xiv—O8—O5^xiv	34.0 (5)
Ca1^ii—O2—B1	128.3 (8)	B3^xiv—O8—O6^xiv	37.2 (7)
Ca1^ii—O2—O1	125.1 (3)	B3^xiv—O8—O7^ii	104.7 (9)
Ca1^ii—O2—O3	96.5 (5)	B3^xiv—O8—O8^x	114.4 (4)
Ca1^ii—O2—O3^viii	83.1 (4)	B3^xiv—O8—O9^xi	110.6 (5)
Ca1^ii—O2—O4^v	98.5 (2)	O1^xv—O8—O3^xiv	98.2 (3)
Ca1^ii—O2—O7^iii	151.8 (5)	O1^xv—O8—O5^xiv	115.7 (3)
Ca1^ii—O2—O9	55.0 (3)	O1^xv—O8—O6^xiv	57.4 (4)
B1—O2—O1	34.1 (5)	O1^xv—O8—O7^ii	162.1 (5)
B1—O2—O3	34.6 (8)	O1^xv—O8—O8^x	69.1 (3)
B1—O2—O3^viii	110.6 (4)	O1^xv—O8—O9^xi	50.4 (3)
B1—O2—O4^v	102.2 (7)	O3^xiv—O8—O5^xiv	60.6 (3)
B1—O2—O7^iii	36.7 (4)	O3^xiv—O8—O6^xiv	61.8 (3)
B1—O2—O9	172.2 (8)	O3^xiv—O8—O7^ii	98.8 (5)
O1—O2—O3	60.1 (4)	O3^xiv—O8—O8^x	83.5 (3)
O1—O2—O3^viii	142.7 (2)	O3^xiv—O8—O9^xi	138.9 (2)
O1—O2—O4^v	69.0 (3)	O5^xiv—O8—O6^xiv	59.5 (4)
O1—O2—O7^iii	59.2 (2)	O5^xiv—O8—O7^ii	78.0 (4)
O1—O2—O9	138.3 (4)	O5^xiv—O8—O8^x	144.0 (4)
O3—O2—O3^viii	96.5 (3)	O5^xiv—O8—O9^xi	105.5 (3)
O3—O2—O4^v	126.0 (3)	O6^xiv—O8—O7^ii	137.5 (6)
O3—O2—O7^iii	59.9 (3)	O6^xiv—O8—O8^x	107.3 (3)
O3—O2—O9	151.0 (6)	O6^xiv—O8—O9^xi	77.7 (3)
O3^viii—O2—O4^v	136.6 (3)	O7^ii—O8—O8^x	107.2 (2)
O3^viii—O2—O7^iii	84.4 (2)	O7^ii—O8—O9^xi	116.8 (3)
O3^viii—O2—O9	76.2 (2)	O8^x—O8—O9^xi	103.5 (5)
O4^v—O2—O7^iii	108.0 (5)	Ca1^ii—O9—B2^xiv	100.1 (10)
O4^v—O2—O9	70.0 (3)	Ca1^ii—O9—O1^xiv	121.3 (5)
O7^iii—O2—O9	144.3 (4)	Ca1^ii—O9—O2	57.1 (3)
B1—O3—B2	61.5 (5)	Ca1^ii—O9—O4^xiv	109.6 (5)
B1—O3—B3	116.2 (7)	Ca1^ii—O9—O5^xiv	64.2 (3)
B1—O3—O1	33.4 (4)	Ca1^ii—O9—O8^vi	127.87 (19)
B1—O3—O2	35.4 (5)	Ca1^ii—O9—O9^xii	109.9 (2)
B1—O3—O2^viii	99.8 (4)	B2^xiv—O9—O1^xiv	35.3 (6)
B1—O3—O5	91.7 (5)	B2^xiv—O9—O2	139.4 (7)
B1—O3—O6	106.0 (4)	B2^xiv—O9—O4^xiv	36.0 (4)
B1—O3—O7^iii	35.9 (3)	B2^xiv—O9—O5^xiv	36.2 (8)
B1—O3—O8^iv	150.4 (4)	B2^xiv—O9—O8^vi	110.4 (7)
B2—O3—B3	61.1 (8)	B2^xiv—O9—O9^xii	115.0 (4)
B2—O3—O1	30.3 (4)	O1^xiv—O9—O2	124.18 (17)
B2—O3—O2	76.5 (3)	O1^xiv—O9—O4^xiv	60.3 (2)
B2—O3—O2^viii	159.6 (4)	O1^xiv—O9—O5^xiv	62.3 (4)
B2—O3—O5	30.9 (5)	O1^xiv—O9—O8^vi	75.2 (3)
B2—O3—O6	76.4 (5)	O1^xiv—O9—O9^xii	122.2 (3)
B2—O3—O7^iii	89.0 (6)	O2—O9—O4^xiv	166.7 (6)
B2—O3—O8^iv	89.2 (4)	O2—O9—O5^xiv	109.4 (4)
B3—O3—O1	90.9 (8)	O2—O9—O8^vi	72.6 (3)
B3—O3—O2	105.3 (3)	O2—O9—O9^xii	104.8 (4)
B3—O3—O2^viii	129.2 (10)	O4^xiv—O9—O5^xiv	60.2 (4)
B3—O3—O5	32.0 (8)	O4^xiv—O9—O8^vi	120.0 (3)
B3—O3—O6	34.8 (4)	O4^xiv—O9—O9^xii	79.3 (3)
B3—O3—O7^iii	149.7 (9)	O5^xiv—O9—O8^vi	129.6 (3)
B3—O3—O8^iv	36.6 (5)	O5^xiv—O9—O9^xii	130.2 (4)
O1—O3—O2	59.8 (3)	O8^vi—O9—O9^xii	94.4 (5)
O1—O3—O2^viii	132.8 (4)

Symmetry codes: (i) −x+1, −y+1, −z+2; (ii) −x+1, −y+1, −z+1; (iii) x, y+1, z; (iv) x, y, z+1; (v) −x, −y+1, −z+1; (vi) x−1, y, z; (vii) x−1, y, z+1; (viii) −x+1, −y+2, −z+1; (ix) −x, −y, −z+1; (x) −x+2, −y+2, −z; (xi) x+1, y, z; (xii) −x, −y+1, −z; (xiii) x, y−1, z; (xiv) x, y, z−1; (xv) x+1, y, z−1.